A kind of cyclohexanol Mead-Bauer recovery system
Technical field
The utility model belongs to rectifying device technical field, and in particular to a kind of cyclohexanol Mead-Bauer recovery system.
Background technology
Cyclohexanol production technique prepares cyclohexene using partial hydrogenation of benzene, through extraction, rectifying, it is refined after cyclohexene pass through
Hydration reaction produces cyclohexanol, and specific production process includes following process:1. hydrogenation process:Using benzene and H2 as raw material, warp
Cross partial hydrogenation reaction generation cyclohexene and hexamethylene;2. extracting rectifying process:Cyclohexene is purified by extraction, rectifying;
3. it is hydrated process:Cyclohexene generates cyclohexanol through hydration reaction;4. cyclohexanol refining step:Finished product is used as after cyclohexanol is refined.
Wherein, to ensure the stability of the product quality of cyclohexanol and system, cyclohexanol treating column and cyclohexanol refine
The discharging any waste liquor amount of tower evaporator is very big, and at present, cyclohexanol waste liquid does not make any processing generally, directly outer at a low price to sell;It is but logical
Cross and analysis and research discovery is carried out to waste liquid, substantial amounts of cyclohexanol is contained in waste liquid, directly will sell and certainly will cause outside waste liquid low price
The waste of this high price chemical products of cyclohexanol.But but there is many difficulty in the cyclohexanol in Recycling of waste liquid:(1) it is basic at present
There is no the recovery system of cyclohexanol waste liquid;(2) cost recovery can not be too high, directly will if the profit of recovery cyclohexanol is no more than
The profit sold outside waste liquid, then the work of devil liquor recovery will be without in all senses for cyclohexanol production enterprise.Therefore have
Necessity designs a kind of cyclohexanol Mead-Bauer recovery system of low energy consumption low cost.
Utility model content
The utility model is directed to problem existing for cyclohexanol devil liquor recovery, there is provided a kind of cyclohexanol Mead-Bauer recovery system.
To achieve the above object, the utility model adopts the following technical scheme that:
A kind of cyclohexanol Mead-Bauer recovery system, including rectifying column, overhead condenser, main feed pipeline, cyclohexanol collecting pipe
Road, heavy constituent collection conduit and jet chimney, the rectifying column bottom are provided with reboiler, and the main feed pipeline is arranged in rectifying
The middle part of tower, the cyclohexanol collection conduit are arranged in the top of rectifying column, and the heavy constituent collection conduit is arranged in rectifying column
Bottom, main feed pipeline is provided with preheater, and the jet chimney is connected to preheater, the cyclohexanol after passing through reboiler
Collection conduit branch is provided with reflux line, and the reflux line is connected to rectifying column, and the position of reflux line access rectifying column
Less than the position of cyclohexanol collection conduit access rectifying column.
Further, the overhead condenser is connected with condensing water conduit, and the main feed pipeline passes through overhead condenser,
And main feed pipeline is located at the lower section of the condensing water conduit.
Further, the rectifying column includes upper and lower two parts, and top is filler portion, and filler portion in rectifying column by filling
Filler is formed, and bottom is column plate portion, and by setting some column plates to form in rectifying column, the main feed pipeline accesses rectifying in column plate portion
Between filler portion and column plate portion, filler portion is provided with upper and lower two sections of packing section, and upper and lower two sections of filler for the position of tower
Extraction pipeline in side is provided between section.
Further, in addition to control system, the control system include tower top pressure control unit, tower top temperature control
Unit and backflow control unit, the tower top pressure control unit include 2# regulating valves and are arranged at the pressure controller of tower top,
The top of the overhead condenser is provided with evacuated tube, and the 2# regulating valves are in evacuated tube, and 2# regulating valves and the pressure
Controller is connected with by the aperture of the Stress control 2# regulating valves of rectifying column tower top.
Further, the tower top temperature control unit includes the 3# regulating valves on condensing water conduit and is arranged at tower
The 1# temperature controllers on top, and 3# regulating valves are connected with 1# temperature controllers with by the temperature control 3# regulating valves of rectifying column tower top
Aperture.
Further, in the cyclohexanol collection conduit after the cyclohexanol collection conduit and reflux line branch location
Provided with 4# regulating valves and flow indicator, the reflux line is provided with 5# regulating valves and 3# flow controllers, the rectifying column
Tower top is provided with 1# fluid level controllers, and the backflow control unit includes the 4# regulating valves, flow indicator, 5# regulating valves, 3#
Flow controller and 1# fluid level controllers, 4# regulating valves are connected with by the Liquid level of rectifying column tower top with 1# fluid level controllers
The aperture of 4# regulating valves, 5# regulating valves are connected with 3# flow controllers to control opening for 5# regulating valves by the flow in reflux line
Degree.
Further, the control system also includes steam flow control unit, and the steam flow control unit includes
8# regulating valves on jet chimney and the 2# temperature controllers located at rectifying column bottom, and 8# regulating valves and 2# temperature controls
Device is connected with by the aperture of the temperature control 8# regulating valves of rectifying column bottom.
Further, the control system also includes side extraction control unit, is set between described upper and lower two sections of packing section
There are 2# flow controllers, the side extraction control unit includes the 2# flow controllers and the 6# on side extraction pipeline
Regulating valve, the 6# regulating valves are connected with 2# flow controllers to be adjusted by the flow control 6# between upper and lower two sections of packing section
Save the aperture of valve.
Further, the control system also includes heavy constituent collection control unit, and the heavy constituent collects control unit
Including the 7# regulating valves in the heavy constituent collection conduit and the 2# fluid level controllers located at the rectifying column bottom, institute
7# regulating valves are stated with 2# fluid level controllers to be connected with by the aperture of the Liquid level 7# regulating valves of rectifying column bottom.
Further, the main feed pipe branch after the preheater has standby feed pipe, the standby charging
The position of pipeline access rectifying column is between upper and lower two sections of packing section.
Further, the heavy constituent collection conduit is provided with decoking unit close to the opening position branch of rectifying column, described de-
Burnt unit includes cyclohexanol recycling pipeline, and one end of the cyclohexanol recycling pipeline is communicated in heavy constituent collection conduit,
The other end is communicated in the bottom of towe opening position of rectifying column, and cyclohexanol recycling pipeline is provided with flash tank, and the flash tank is through pipe
Road, which is connected between vavuum pump and flash tank and vavuum pump, is provided with vacuum breaker, and the bottom of flash tank recombinates subtube through remnants
It is communicated to heavy constituent collection conduit;In the communicating position and remaining restructuring of cyclohexanol recycling pipeline and heavy constituent collection conduit
4# stop valves are provided between the communicating position of subtube and heavy constituent collection conduit.
The beneficial effects of the utility model are as follows:
(1) charging heat exchange, energy consumption is saved:The main feed pipeline passes through overhead condenser, and main feed pipeline is located at institute
The lower section of condensing water conduit is stated, the gas phase temperature of rectifying column tower top is higher, it is necessary to the condensation that cools obtains overhead distillate, traditional
Cooling method is the cooling water temperature that is passed through of overhead condenser, and the utility model the waste liquid in main feed pipeline is also served as it is cold
But medium, and main feed pipeline is located to the lower section of condensing water conduit, the gas phase of rectifying column tower top touches main feed pipe first
Road, exchanged heat with waste liquid, while gas phase cools, waste liquid heating, made the best of both worlds, then gas phase continues up and cooling water pipe
Road contacts, and condensation obtains overhead distillate;
(2) steam heat-exchanging, energy consumption is saved:The utility model is made full use of to the heat of steam, first by again
The liquid phase heat exchange in device, with reboiler is boiled, promotes the gasification of liquid phase in reboiler, then steam enters preheater, pre- to entering
After the waste liquid of hot device is preheated, finally enter with the waste liquid after preheating in rectifying column;
(3) backflow control is fine, and product purity is high:It is that product is pure that whether recovery, which has one of important indicator of economic value,
Degree, the utility model realize that cyclohexanol is collected flow control and controlled with return flow, wherein cyclohexanol by the control unit that flows back
Flow associates control with tower top liquid level, and the double control of return flow and cyclohexanol flow is protected so as to obtain suitable reflux ratio
Product purity has been demonstrate,proved, has improved the economic value of cyclohexanol devil liquor recovery;
(4) Application of composite in rectifying inner-tower filling material portion and column plate portion:This design side of rectifying column described in the utility model
Formula make it that gas-liquid two-phase distribution is more uniform, efficiently utilizes gas-phase space, and mass-transfer efficiency increases, and improving, product is pure
In the case of degree, capacity of returns can be also reduced, so as to reduce energy consumption;
(5) extraction design in side can play multiple functions according to different demands, for example, can will between tower top light component and
Intermediate species between bottom of towe heavy constituent isolates system in time, improves separative efficiency, while can also obtain the pair of intermediate species
Product;Furthermore when intermediate species has enrichment between upper and lower packing section, the richness to obtain the enriched composition product or disappearing
Collect influence of the component to tower both ends product, set side to produce passage, the enriched composition is produced in time;
(6) control system:The utility model employs the control system that multiple control units constitute whole distillation process,
The control to each parameter such as rectification temperature, pressure, liquid level, flow, reflux ratio is realized, reduces operation window, it is ensured that process exists
Carried out under lowest energy consumption;
(7) double design of main feed passage and standby feeding-passage:The convenient elasticity adjustment of mode of this two bursts of chargings
Rectifying section and stripping section, to reach the purpose for reducing energy consumption and improving product purity;Meanwhile in the cyclohexanol production of different batches
In, the component of obtained cyclohexanol waste liquid is although identical, but composition has differences, and the cyclohexanol that different batches are obtained gives up
When liquid is separated in same rectifying column, to avoid the energy consumption that increase separates, then it can be added respectively in each suitable position.
To sum up, the utility model provides a kind of cyclohexanol Mead-Bauer recovery system, can not only realize the recovery of cyclohexanol,
And obtained cyclohexanol product high purity more than 95%, while the byproduct of heavy constituent is obtained, the hexamethylene in the heavy constituent
Alcohol residual volume is less than 2.0%, and directly outer compared to waste liquid to sell, economic value is high, meanwhile, recovery system described in the utility model
Elastic adjustment space is big, can adapt to the cyclohexanol waste liquid of different compositions and the product demand of different purity, and application value is high, and
And the utility model passes through the flexible arrangement of heat exchanger components and the Fine design of control system so that whole recovery system exists
Run under lowest energy consumption, significantly reduce cost recovery, promotional value is high.
Brief description of the drawings
Fig. 1 is the structural representation of cyclohexanol Mead-Bauer recovery system described in embodiment 1;
1st, filler portion;2nd, column plate portion;3rd, tower top adopts batch can;30th, 1# fluid level controllers;
10th, pressure controller;11st, 1# temperature controllers;12nd, 1# temperature indicators;13rd, liquid level alarm;14th, 2# flows
Controller;15th, 2# temperature indicators;
20th, reboiler;21st, 2# temperature controllers;22nd, 2# fluid level controllers;
40th, main feed pipeline;400th, 1# regulating valves;401st, 1# flow controllers;402nd, 1# stop valves;
41st, overhead condenser;410th, evacuated tube;4100th, 2# regulating valves;411st, condensing water conduit;4110th, 3# regulating valves;
42nd, preheater;43rd, 1# pumps;44th, standby feed pipe;440th, 2# stop valves;
50th, 2# pumps;51st, cyclohexanol collection conduit;510th, 4# regulating valves;511st, flow indicator;52nd, reflux line;
520th, 5# regulating valves;521st, 3# flow controllers;
6th, side extraction pipeline;60th, 3# pumps;61st, 1# coolers;62nd, 6# regulating valves;63rd, 3# stop valves;
7th, heavy constituent collection conduit;70th, 4# pumps;71st, 7# regulating valves;72nd, 2# coolers;
8th, jet chimney;80th, 8# regulating valves;
9th, flash tank;900th, cyclohexanol recycling pipeline;901st, 5# pumps;902nd, vacuum breaker;903rd, vavuum pump;904、
Remnants restructuring subtubes;905th, 4# stop valves;
Fig. 2 is the structural representation of cyclohexanol Mead-Bauer recovery system described in embodiment 2.
Embodiment
In order that technical purpose of the present utility model, technical scheme and beneficial effect are clearer, below in conjunction with the accompanying drawings and
Specific embodiment is further illustrated to the technical solution of the utility model.
Embodiment 1
As shown in figure 1, a kind of cyclohexanol Mead-Bauer recovery system, including rectifying column, main feed pipeline 40,2# cyclohexanol are collected
Pipeline 51, heavy constituent collection conduit 7 and jet chimney 8, the rectifying column tower top are disposed with tower top and adopt batch can 3 from bottom to top
With overhead condenser 41, the overhead condenser 41 is connected with condensing water conduit 411, and the main feed pipeline 40 is cold through tower top
Condenser 41, and main feed pipeline 40 is located at the lower section of the condensing water conduit 411, and main feed pipeline 40 is arranged in rectifying column
Middle part, 1# pumps 43 for feeding are provided with before overhead condenser 41 on main feed passage and in overhead condenser 41 and 1# pumps
1# regulating valves 400 and 1# flow controllers 401 are provided between 43, the 1# regulating valves 400 are connected with 1# flow controllers 401
To control the aperture of 1# regulating valves 400 by the flow in main feed pipeline 40, on main feed passage after overhead condenser 41
Provided with preheater 42, rectifying column bottom is provided with reboiler 20, and the 2# cyclohexanol collection conduit 51 is arranged in tower top and adopts batch can 3,
And 2# cyclohexanol collection conduit 51 is provided with 2# pumps 50 close to the opening position of rectifying column, the heavy constituent collection conduit 7 is arranged in essence
The bottom of tower is evaporated, and heavy constituent collection conduit 7 is provided with 4# pumps 70 close to the opening position of rectifying column, the jet chimney 8 is through again
Preheater 42 is connected to after boiling device 20, the branch of 2# cyclohexanol collection conduit 51 is provided with reflux line 52, the reflux line
52 are connected to rectifying column tower top, and rectifying column is accessed in the position that reflux line 52 accesses rectifying column less than 2# cyclohexanol collection conduit 51
Position.
Further, the rectifying column includes upper and lower two parts, and top is filler portion 1, and filler portion 1 in rectifying column by filling out
Casting resin is formed, and bottom is column plate portion 2, and by setting some column plates to form in rectifying column, the column plate is led for single overflow in column plate portion 2
To trapezoidal float valve tray, column plate spacing is 300-600mm, and float valve can improve column plate with the upper and lower free floating of change of gas velocity
Operating flexibility, reduce the pressure drop of column plate, while have compared with high tower plate efficiency;The main feed pipeline 40 accesses the position of rectifying column
Setting between filler portion 1 and column plate portion 2, filler portion 1 is provided with upper and lower two sections of packing section, and the filler of upper packing section is expanded metals
Filler, expanded metals packed height are about 3-5m, and the filler of lower packing section is perforated plate corrugated filler, and perforated plate corrugated filler height is about
For 2-4m;And extraction pipeline 6 in side is provided between upper and lower two sections of packing section, the side produces pipeline 6 close to the position of rectifying column
Place is sequentially provided with 3# stop valves 63 and 3# pumps 60, and there is standby feed pipe in the branch of main feed pipeline 40 after the preheater 42
Road 44, the standby feed pipe 44 accesses the position of rectifying column between upper and lower two sections of packing section, and main feed pipeline
40 and standby feed pipe 44 be respectively equipped with 1# stop valves 402 and 2# stop valves 440 close to the opening position of rectifying column.In addition, upper,
Rectifying column between lower two sections of packing section is provided with 1# temperature indicators 12 and liquid level alarm 13, filler portion 1 and column plate portion 2
Between rectifying column be provided with 2# temperature indicators 15.
Further, the utility model also includes control system, and the control system includes tower top pressure control unit, tower
Temperature control unit and backflow control unit are pushed up, the tower top pressure control unit includes 2# regulating valves 4100 and is arranged at tower top
Pressure controller 10, the top of the overhead condenser 41 is provided with evacuated tube 410, and the 2# regulating valves 4100 are located at evacuated tube
On 410, and 2# regulating valves 4100 are connected with the pressure controller 10 with by the Stress control 2# regulating valves of rectifying column tower top
4100 aperture, top gaseous phase produce condensate liquid and fixed gas in the presence of overhead condenser 41, and fixed gas passes through evacuated tube
410 discharge to adjust tower top pressure.
Further, the tower top temperature control unit includes the He of 3# regulating valves 4110 on condensing water conduit 411
The 1# temperature controllers 11 of tower top are arranged at, and 3# regulating valves 4110 are connected with by rectifying column tower top with 1# temperature controllers 11
Temperature control 3# regulating valves 4110 aperture.
Further, the 2# cyclohexanol after the 2# cyclohexanol collection conduit 51 and the branch location of reflux line 52 is received
Collection pipeline 51 is provided with 4# regulating valves 510 and flow indicator 511, and the reflux line 52 is provided with 5# regulating valves 520 and 3#
Flow controller 521, the rectifying column tower top are provided with 1# fluid level controllers 30, and the backflow control unit is adjusted including the 4#
Valve 510, flow indicator 511,5# regulating valves 520,3# flow controllers 521 and 1# fluid level controllers 30,4# regulating valves 510
Be connected with 1# fluid level controllers 30 with by the aperture of the Liquid level 4# regulating valves 510 of rectifying column tower top, 5# regulating valves 520 with
3# flow controllers 521 are connected to control the aperture of 5# regulating valves 520 by the flow in reflux line 52.
Further, the control system also includes steam flow control unit, and the steam flow control unit includes
8# regulating valves 80 on jet chimney 8 and the 2# temperature controllers 21 located at rectifying column bottom, and 8# regulating valves 80 and 2#
Temperature controller 21 is connected with by the aperture of the temperature control 8# regulating valves 80 of rectifying column bottom.
Further, the control system also includes side extraction control unit, is set between described upper and lower two sections of packing section
There are 2# flow controllers 14, the side extraction control unit includes the 2# flow controllers 14 and produces pipeline 6 located at side
On 6# regulating valves 62, the 6# regulating valves 62 are connected with by between upper and lower two sections of packing section with 2# flow controllers 14
The aperture of flow control 6# regulating valves 62, the side extraction passage after 6# regulating valves 62 is provided with 1# coolers 61, for cold
But the intermediate species of side extraction.
Further, the control system also includes heavy constituent collection control unit, and the heavy constituent collects control unit
Including the 7# regulating valves 71 in the heavy constituent collection conduit 7 and the 2# fluid level controllers located at the rectifying column bottom
22, the 7# regulating valves 71 are connected with 2# fluid level controllers 22 with opening by the Liquid level 7# regulating valves 71 of rectifying column bottom
Degree, the heavy constituent collection conduit 7 after 7# regulating valves 71 are provided with 2# coolers 72, the cooling for heavy constituent.
Operation principle of the present utility model is as follows:
(after testing, key component is as follows in cyclohexanol waste liquid W L by cyclohexanol waste liquid W L:Cyclohexanol 64.00wt%, hexichol
Ether 11.7wt%, hexyl ether 24.2wt%) it is pumped into through 1# pumps 43 in main feed pipeline 40, in the overhead condenser 41 and rectifying
Entered after the heat exchange of column overhead gas phase in preheater 42,1300kPa saturated vapor SS is delivered to reboiler by jet chimney 8
20, after saturated vapor exchanges heat with the liquid phase in reboiler 20, into preheater 42, exchanged heat with the cyclohexanol waste liquid of preheater 42,
Then saturated vapor and cyclohexanol waste liquid are delivered in rectifying column by main feed pipeline 40 together, and feeding temperature is 70 DEG C of 50-,
Distillation process is carried out, tower top pressure control is controlled in 1.5- in 15-50KPa, tower top temperature control in 135 DEG C of 110-, reflux ratio
3, the condensation in overhead condenser 41 of top gaseous phase caused by rectifying obtains condensate liquid, the cooling water CW that overhead condenser 41 is passed through
At 32-42 DEG C, condensate liquid is stored in tower top and adopted in batch can 3 temperature control, and in the presence of 2# pumps 50, condensate liquid is received by cyclohexanol
Collector conveys, and partial condensation liquid is back to rectifying column tower top as phegma by reflux line 52, and remaining condensate liquid collects storage
In tank, cyclohexanol product L is produced;Intermediate species caused by rectifying is enriched between upper and lower packing section, and 3# stop valves 63 are in normal
Closed state, the enrichment situation of intermediate species can be learnt by liquid level alarm 13, when intermediate species enrichment reaches to a certain degree
When, 3# stop valves 63 and 3# pumps 60 are opened, in the presence of 3# pumps 60, intermediate species is pumped to side extraction pipeline 6, passes through simultaneously
2# flow controllers 14 change the aperture of 6# regulating valves 62, and so as to adjust the flow of side extraction passage, intermediate species C is cold through 1#
But device 61 is collected after being cooled to 50-60 DEG C;Heavy constituent H caused by rectifying is in the presence of 4# pumps 70, in heavy constituent collection conduit
Convey in 7, collected after being cooled to 50-60 DEG C via 2# coolers 72.After testing, cyclohexanol product L purity is 99.0wt%,
Heavy constituent H key component is as follows:Diphenyl ether 20.60wt%, hexyl ether 74.20wt%, the content of cyclohexanol is as little as
0.28wt%.In distillation process, control system co-ordination described in the utility model, control flow in each pipeline,
The parameters such as temperature, pressure, liquid level in rectifying column, ensure that distillation process is carried out under conditions of low energy consumption, high product purity, have
Addressed before body control mode, here is omitted.
Embodiment 2
As shown in Fig. 2 the difference of embodiment 2 and embodiment 1 is, the heavy constituent collection conduit 7 is close to rectifying
The opening position branch of tower is provided with decoking unit, and the decoking unit includes cyclohexanol recycling pipeline 900, and the cyclohexanol is again
One end of recovery channel 900 is communicated in heavy constituent collection conduit 7, and the other end is communicated in the bottom of towe opening position of rectifying column, and ring
Hexanol recycling pipeline 900 is provided with flash tank 9, the flash tank 9 through pipeline be connected to vavuum pump 903 and flash tank 9 with it is true
Vacuum breaker 902 is provided between empty pump 903, the bottom of flash tank 9 is communicated to heavy constituent through remnants restructuring subtubes 904 and collected
Pipeline 7, in the communicating position and remaining restructuring subtube 904 of cyclohexanol recycling pipeline 900 and heavy constituent collection conduit 7
4# stop valves 905 are provided between the communicating position of heavy constituent collection conduit 7.
The effect of decoking unit is:When detecting in heavy constituent H of the rectifying tower bottom through arranging outside heavy constituent collection conduit 7
Hexamethylene alcohol content more than 5% when, to avoid the waste of the part cyclohexanol, improve the rate of recovery, spy is provided with decoking unit:
4# stop valves 905 are closed, open vavuum pump 903, and pass through the vacuum inside the regulation of vacuum breaker 902 flash tank 9 to 5-
10kPa, then the heavy constituent in heavy constituent collection conduit 7 via cyclohexanol recycling pipeline 900 enter flash tank 9, after flash distillation,
The cyclohexanol of gas phase is cooled to 60-80 DEG C or so after supercooling and delivers to rectifying tower bottom, remaining heavy constituent by 5# pumps 901
The content of middle cyclohexanol is 0.5-1%, is back to through remnants restructuring subtubes 904 in heavy constituent collection conduit 7, then outer to arrange;
The cyclohexanol in heavy constituent can be effectively recycled by the method, economic benefit is optimal.
It should be noted last that:Above-described embodiment is merely to illustrate and unrestricted the technical solution of the utility model, is appointed
The equivalent substitution and do not depart from the modification of the spirit and scope of the utility model or local replacement what is carried out to the utility model, its is equal
It should cover within the scope of the utility model claims protection.