CN107261540A - A kind of cyclohexanol Mead-Bauer recovery system - Google Patents

A kind of cyclohexanol Mead-Bauer recovery system Download PDF

Info

Publication number
CN107261540A
CN107261540A CN201710535599.2A CN201710535599A CN107261540A CN 107261540 A CN107261540 A CN 107261540A CN 201710535599 A CN201710535599 A CN 201710535599A CN 107261540 A CN107261540 A CN 107261540A
Authority
CN
China
Prior art keywords
cyclohexanol
rectifying column
regulating valves
collection conduit
heavy constituent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710535599.2A
Other languages
Chinese (zh)
Inventor
乔思怀
赵铎
陈聚良
史红军
卢磊
张乐
孟保勋
李延民
邹柯柯
杨莉
郭卫东
欧玲
张佩兰
段文蕊
陈聪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HENAN SHENMA NYLON CHEMICAL CO Ltd
Original Assignee
HENAN SHENMA NYLON CHEMICAL CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HENAN SHENMA NYLON CHEMICAL CO Ltd filed Critical HENAN SHENMA NYLON CHEMICAL CO Ltd
Priority to CN201710535599.2A priority Critical patent/CN107261540A/en
Publication of CN107261540A publication Critical patent/CN107261540A/en
Pending legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42Regulation; Control
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42Regulation; Control
    • B01D3/4205Reflux ratio control splitter
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention provides a kind of cyclohexanol Mead-Bauer recovery system, including rectifying column, overhead condenser, main feed pipeline, cyclohexanol collection conduit, heavy constituent collection conduit and jet chimney, the rectifying column bottom is provided with reboiler, the main feed pipeline is arranged in the middle part of rectifying column, the cyclohexanol collection conduit is arranged in the top of rectifying column, the heavy constituent collection conduit is arranged in the bottom of rectifying column, main feed pipeline is provided with preheater, the jet chimney after reboiler by being connected to preheater, the cyclohexanol collection conduit branch is provided with reflux line, the reflux line is connected to rectifying column, and the position of reflux line access rectifying column accesses the position of rectifying column less than cyclohexanol collection conduit.The present invention can not only realize the recovery of cyclohexanol, and obtained cyclohexanol product purity is high, while obtaining the byproduct of heavy constituent and intermediate species, directly outer compared to waste liquid to sell, economic value is high.

Description

A kind of cyclohexanol Mead-Bauer recovery system
Technical field
The invention 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 lead to Hydration reaction production cyclohexanol is crossed, specific production process includes following process:1. hydrogenation process:Using benzene and H2 as raw material, By partial hydrogenation reaction generation cyclohexene and hexamethylene;2. extracting rectifying process:Cyclohexene is carried by extraction, rectifying It is pure;3. it is hydrated process:Cyclohexene generates cyclohexanol through hydration reaction;4. cyclohexanol refining step:It is used as into after cyclohexanol is refined Product.
Wherein, to ensure the product quality of cyclohexanol and the stability of system, cyclohexanol treating column and cyclohexanol are refined The discharging any waste liquor amount of tower evaporator is very big, at present, and cyclohexanol waste liquid does not make any processing generally, directly outer at a low price to sell;But it is logical Cross and waste liquid is carried out to contain substantial amounts of cyclohexanol in analysis and research discovery, 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) current root This recovery system without cyclohexanol waste liquid;(2) cost recovery can not be too high, if reclaiming the profit of cyclohexanol no more than straight Connect the profit that will be sold outside waste liquid, then the work of devil liquor recovery will be without in all senses for cyclohexanol production enterprise.Cause This is necessary to design a kind of cyclohexanol Mead-Bauer recovery system of low energy consumption low cost.
The content of the invention
There is provided a kind of cyclohexanol Mead-Bauer recovery system for problem of the invention for the presence of cyclohexanol devil liquor recovery.
To achieve the above object, the present invention is adopted the following technical scheme that:
A kind of cyclohexanol Mead-Bauer recovery system, including rectifying column, overhead condenser, main feed pipeline, cyclohexanol collection conduit, Heavy constituent collection conduit and jet chimney, the rectifying column bottom are provided with reboiler, and the main feed pipeline is arranged in rectifying column Middle part, the cyclohexanol collection conduit is 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 reflux line accesses the position of rectifying column Less than the position that cyclohexanol collection conduit accesses rectifying column.
Further, the overhead condenser is connected with condensing water conduit, and the main feed pipeline passes through overhead condensation Device, 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 is filled in rectifying column Filler is constituted, and bottom is column plate portion, and column plate portion sets some column plates to constitute in rectifying column, the main feed pipeline access essence The position for evaporating tower is located 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 are filled out Expect to produce pipeline provided with side between section.
Further, in addition to control system, the control system includes tower top pressure control unit, tower top temperature control Unit processed and backflow control unit, the tower top pressure control unit include 2# regulating valves and are arranged at the Stress control of tower top Device, the top of the overhead condenser is provided with evacuated tube, the 2# regulating valves in evacuated tube, and 2# regulating valves with it is described 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 The 1# temperature controllers of tower top, and 3# regulating valves be connected with 1# temperature controllers with by the temperature control 3# of rectifying column tower top adjust Save the aperture of valve.
Further, the cyclohexanol collection conduit after the cyclohexanol collection conduit and reflux line branch location 4# regulating valves and flow indicator are provided with, the reflux line is provided with 5# regulating valves and 3# flow controllers, the rectifying Column overhead be provided with 1# fluid level controllers, the backflow control unit include the 4# regulating valves, flow indicator, 5# regulating valves, 3# flow controllers 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 is controlled, 5# regulating valves are connected with 3# flow controllers with the flow control 5# regulations in reflux line The aperture of valve.
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 processed is connected with by the aperture of the temperature control 8# regulating valves of rectifying column bottom.
Further, the control system is also included between side extraction control unit, described upper and lower two sections of packing section Provided with 2# flow controllers, the side extraction control unit includes the 2# flow controllers and on side extraction pipeline 6# regulating valves, the 6# regulating valves be connected with 2# flow controllers between upper and lower two sections of packing section flow control The aperture of 6# regulating valves.
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 located between upper and lower two sections of packing section.
Further, the heavy constituent collection conduit has installed decoking unit close to the position punishment 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 at the bottom of towe 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 is in charge of through remnants restructuring Road is communicated to heavy constituent collection conduit;In cyclohexanol recycling pipeline and the communicating position and remnants of heavy constituent collection conduit Recombinate and 4# stop valves are provided between subtube and the communicating position of heavy constituent collection conduit.
Beneficial effects of the present invention are as follows:
(1) charging heat exchange, saves energy consumption:The main feed pipeline passes through overhead condenser, and main feed pipeline is positioned at described cold The lower section of solidifying waterpipe, the gas phase temperature of rectifying column tower top is higher, it is necessary to which the condensation that cools obtains overhead distillate, traditional drop Warm mode is the cooling water temperature that overhead condenser is passed through, and the waste liquid in main feed pipeline is also served as cooling and is situated between by the present invention Matter, 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 pipeline first, Exchanged heat with waste liquid, while gas phase cools, waste liquid heating makes the best of both worlds, then gas phase is continued up and cooling water pipeline Contact, condensation obtains overhead distillate;
(2) steam heat-exchanging, saves energy consumption:The present invention is made full use of to the heat of steam, first by reboiler, with Liquid phase heat exchange in reboiler, promotes the gasification of liquid phase in reboiler, then steam enters preheater, to entering preheater After waste liquid is preheated, finally enter with the waste liquid after preheating in rectifying column;
(3) backflow control is fine, and product purity is high:Whether recovery has one of important indicator of economic value to be product purity, The present invention by the control unit that flows back, realize cyclohexanol collect flow control with return flow control, wherein cyclohexanol flow with The double control of the association control of tower top liquid level, return flow and cyclohexanol flow is so as to obtain suitable reflux ratio, it is ensured that production Product purity, improves 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 method of rectifying column of the present invention makes to bring about the desired sensation The distributed mutually of liquid two is more uniform, efficiently utilizes gas-phase space, and mass-transfer efficiency increases, and is improving the feelings of product purity Under condition, capacity of returns can be also reduced, so as to reduce energy consumption;
(5) extraction design in side can play a variety of functions according to different demands, for example can be by between tower top light component and bottom of towe Intermediate species between heavy constituent isolates system in time, separative efficiency is improved, while can also obtain the by-product of intermediate species Product;Furthermore, when intermediate species has enrichment between packing section up and down, the richness to obtain the enriched composition product or disappearing Collect influence of the component to tower two ends product, set side to produce passage, the enriched composition is produced in time;
(6) control system:Present invention employs the control system that multiple control units constitute whole distillation process, realize Control to each parameter such as rectification temperature, pressure, liquid level, flow, reflux ratio, reduces operation window, it is ensured that process is in most low energy Consumption is lower to be carried out;
(7) double design of main feed passage and standby feeding-passage:The convenient elasticity adjustment rectifying of mode of this two bursts of chargings Section and stripping section, with the purpose for reaching reduction energy consumption and improving product purity;Meanwhile, in the cyclohexanol production of different batches, The component of obtained cyclohexanol waste liquid is although identical, but composition has differences, the cyclohexanol waste liquid that different batches are obtained When being separated in same rectifying column, to avoid the energy consumption that increase is separated, then it can be added respectively in each suitable position.
To sum up, the invention provides a kind of cyclohexanol Mead-Bauer recovery system, the recovery of cyclohexanol can not only be realized, and And obtained cyclohexanol product high purity more than 95%, while the byproduct of heavy constituent is obtained, the cyclohexanol in the heavy constituent Residual volume is less than 2.0%, and directly outer compared to waste liquid to sell, economic value is high, meanwhile, the elasticity of recovery system of the present invention 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, moreover, Flexible arrangement and the Fine design of control system that the present invention passes through heat exchanger components so that whole recovery system is in most low energy Consumption is lower to be run, and significantly reduces cost recovery, promotional value is high.
Brief description of the drawings
Fig. 1 is the structural representation of embodiment 1;
Fig. 2 is the structural representation of embodiment 2;
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 control Device processed;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;520、5# Regulating valve;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;904th, it is residual Remaining restructuring subtube;905th, 4# stop valves.
Embodiment
In order that the technical purpose of the present invention, technical scheme and beneficial effect are clearer, below in conjunction with the accompanying drawings and specifically Embodiment is further illustrated to technical scheme.
Embodiment 1
As shown in figure 1, a kind of cyclohexanol Mead-Bauer recovery system, including rectifying column, main feed pipeline 40,2# cyclohexanol collecting pipes Road 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 passes 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 Being provided with the middle part of tower, main feed passage before overhead condenser 41 is used for the 1# pumps 43 of charging and in overhead condenser 41 1# regulating valves 400 and 1# flow controllers 401, the 1# regulating valves 400 and 1# flow controllers are provided between 1# pumps 43 401, which are connected, is controlled on the aperture of 1# regulating valves 400, main feed passage with the flow in main feed pipeline 40 in overhead condensation Preheater 42 is provided with after device 41, rectifying column bottom is provided with reboiler 20, and the 2# cyclohexanol collection conduit 51 is arranged in tower top Batch can 3 is adopted, and 2# cyclohexanol collection conduit 51 is provided with 2# pumps 50, the heavy constituent collection conduit 7 at the position of rectifying column The bottom of rectifying column is arranged in, and heavy constituent collection conduit 7 is provided with 4# pumps 70, the steam pipe at the position of rectifying column Road 8 passes through and preheater 42 is connected to after reboiler 20, and the branch of 2# cyclohexanol collection conduit 51 is provided with reflux line 52, institute State reflux line 52 and be connected to rectifying column tower top, the position of the access rectifying column of reflux line 52 is less than 2# cyclohexanol collection conduits The position of 51 access rectifying columns.
Further, the rectifying column includes upper and lower two parts, and top is filler portion 1, and filler portion 1 is filled out in rectifying column Casting resin is constituted, and bottom is column plate portion 2, and column plate portion 2 sets some column plates to constitute in rectifying column, and the column plate is single overflow Guiding ladder-shaped float valve column plate, column plate spacing be 300-600mm, float valve can with gas velocity the upper and lower free floating of change, improve The operating flexibility of column plate, the pressure drop for reducing column plate, while having compared with high tower plate efficiency;The main feed pipeline 40 accesses rectifying The position of tower is located between filler portion 1 and column plate portion 2, and filler portion 1 is provided with upper and lower two sections of packing section, the filler of upper packing section For expanded metals filler, expanded metals packed height is about 3-5m, and the filler of lower packing section is perforated plate corrugated filler, perforated plate corrugated filler Highly it is about 2-4m;And pipeline 6 is produced provided with side between upper and lower two sections of packing section, the side extraction pipeline 6 is close to essence Evaporate and 3# stop valves 63 and 3# pumps 60 are sequentially provided with the position of tower, the branch of main feed pipeline 40 after the preheater 42 Have a standby feed pipe 44, the position of the standby access of feed pipe 44 rectifying column be located at upper and lower two sections packing section it Between, and 1# stop valves 402 are respectively equipped with the position of rectifying column for main feed pipeline 40 and standby feed pipe 44 and 2# is cut Only valve 440.In addition, the rectifying column between upper and lower two sections of packing section is provided with 1# temperature indicators 12 and liquid level alarm 13, the rectifying column between filler portion 1 and column plate portion 2 is provided with 2# temperature indicators 15.
Further, present invention additionally comprises control system, the control system includes tower top pressure control unit, tower top Temperature control unit and backflow control unit, the tower top pressure control unit include 2# regulating valves 4100 and are 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 emptying On pipe 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 produces 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 Collection conduit 51 is provided with 4# regulating valves 510 and flow indicator 511, and the reflux line 52 is provided with the He of 5# regulating valves 520 3# flow controllers 521, the rectifying column tower top is provided with 1# fluid level controllers 30, and the backflow control unit includes the 4# Regulating valve 510, flow indicator 511,5# regulating valves 520,3# flow controllers 521 and 1# fluid level controllers 30,4# regulations Valve 510 is 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 are connected with 3# flow controllers 521 with the aperture of the flow control 5# regulating valves 520 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 is also included between side extraction control unit, described upper and lower two sections of packing section Provided with 2# flow controllers 14, the side extraction control unit includes the 2# flow controllers 14 and produces pipeline located at side 6# regulating valves 62 on 6, the 6# regulating valves 62 are connected between upper and lower two sections of packing section with 2# flow controllers 14 Flow control 6# regulating valves 62 aperture, the side extraction passage after 6# regulating valves 62 is provided with 1# coolers 61, is used for The intermediate species of cold 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 is provided with 2# coolers 72, the cooling for heavy constituent.
The operation principle of the present invention 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%, diphenyl 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 column Entered after top gaseous phase heat exchange in preheater 42,1300kPa saturated vapor SS is delivered to reboiler 20 by jet chimney 8, Saturated vapor with the cyclohexanol waste liquid of preheater 42 with after the liquid phase heat exchange in reboiler 20, into preheater 42, exchanging heat, so Saturated vapor and cyclohexanol waste liquid are delivered in rectifying column by main feed pipeline 40 together afterwards, and feeding temperature is 70 DEG C of 50-, is entered Row distillation process, tower top pressure control is in 15-50KPa, and tower top temperature control is in 135 DEG C of 110-, and reflux ratio is controlled in 1.5-3, The top gaseous phase that rectifying is produced condensation in overhead condenser 41 obtains condensate liquid, the cooling water CW that overhead condenser 41 is passed through Temperature control is at 32-42 DEG C, and condensate liquid is stored in tower top and adopted in batch can 3, and in the presence of 2# pumps 50, condensate liquid is by cyclohexanol Collecting pipe is conveyed, and partial condensation liquid is back to rectifying column tower top as phegma by reflux line 52, and remaining condensate liquid is collected In storage tank, cyclohexanol product L is produced;The intermediate species that rectifying is produced is enriched between packing section up and down, at 3# stop valves 63 In normally off, the enrichment situation of intermediate species can be learnt by liquid level alarm 13, when intermediate species enrichment reaches necessarily During degree, 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, together When change the aperture of 6# regulating valves 62 by 2# flow controllers 14, so as to adjust the flow that side produces passage, intermediate species C Collected after being cooled to 50-60 DEG C through 1# coolers 61;The heavy constituent H that rectifying is produced is received in the presence of 4# pumps 70 in heavy constituent Collect in pipeline 7 and convey, be cooled to after 50-60 DEG C and collect 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 As little as 0.28wt%.In distillation process, control system co-ordination of the present invention, control flow in each pipeline, The parameters such as temperature, pressure, liquid level in rectifying column, it is ensured that distillation process is carried out under conditions of low energy consumption, high product purity, Addressed before specific 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 column Position punishment has installed decoking unit, and the decoking unit includes cyclohexanol recycling pipeline 900, the cyclohexanol recycling One end of pipeline 900 is communicated in heavy constituent collection conduit 7, and the other end is communicated at the bottom of towe position of rectifying column, and cyclohexanol Recycling pipeline 900 is provided with flash tank 9, and the flash tank 9 is connected to vavuum pump 903 and flash tank 9 and vavuum pump through pipeline Vacuum breaker 902 is provided between 903, the bottom of flash tank 9 is communicated to heavy constituent collecting pipe through remnants restructuring subtubes 904 Road 7, cyclohexanol recycling pipeline 900 and heavy constituent collection conduit 7 communicating position and remaining restructuring subtube 904 with 4# stop valves 905 are provided between the communicating position of heavy constituent collection conduit 7.
The effect of decoking unit is:When detecting heavy constituent H of the rectifying tower bottom through the outer row of heavy constituent collection conduit 7 In 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 list Member:4# stop valves 905 are closed, vavuum pump 903 are opened, and the vacuum inside flash tank 9 is adjusted by vacuum breaker 902 To 5-10kPa, then the heavy constituent in heavy constituent collection conduit 7 is via the entrance flash tank 9 of cyclohexanol recycling pipeline 900, sudden strain of a muscle After steaming, the cyclohexanol of gas phase is cooled to 60-80 DEG C or so after supercooling and delivers to rectifying tower bottom by 5# pumps 901, remaining The content of cyclohexanol is 0.5-1% in heavy constituent, is back to through remnants restructuring subtubes 904 in heavy constituent collection conduit 7, so It is outer afterwards 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 the technical scheme being not intended to limit the present invention, any right Equivalent substitution and do not depart from the modification of spirit and scope of the invention or locally replace that the present invention is carried out, it all should cover at this Within the scope of invention right is claimed.

Claims (10)

1. a kind of cyclohexanol Mead-Bauer recovery system, including rectifying column, overhead condenser, main feed pipeline, cyclohexanol collection conduit, Heavy constituent collection conduit and jet chimney, the rectifying column bottom are provided with reboiler, and the main feed pipeline is arranged in rectifying column Middle part, the cyclohexanol collection conduit is arranged in the top of rectifying column, and the heavy constituent collection conduit is arranged in rectifying column Bottom, it is characterised in that:Main feed pipeline be provided with preheater, the jet chimney by being connected to preheater after reboiler, The cyclohexanol collection conduit branch is provided with reflux line, and the reflux line is connected to rectifying column, and reflux line access essence The position for evaporating tower accesses the position of rectifying column less than cyclohexanol collection conduit.
2. cyclohexanol Mead-Bauer recovery system according to claim 1, it is characterised in that:The overhead condenser is connected with cold Solidifying waterpipe, the main feed pipeline passes through overhead condenser, and main feed pipeline is located at the lower section of the condensing water conduit.
3. cyclohexanol Mead-Bauer recovery system according to claim 2, it is characterised in that:The rectifying column includes upper and lower two Part, top is filler portion, and filler portion fills filler in rectifying column and constituted, and bottom is tower tray portion, and tower tray portion is in rectifying column Some column plates are set to constitute, the position of the main feed pipeline access rectifying column is located between filler portion and column plate portion, filler portion Pipeline is produced provided with side is provided between upper and lower two sections of packing section, and upper and lower two sections of packing section.
4. the cyclohexanol Mead-Bauer recovery system according to claims 1 to 3, it is characterised in that:Also include control system, it is described Control system includes tower top pressure control unit, tower top temperature control unit and backflow control unit, the tower top pressure control Unit includes 2# regulating valves and is arranged at the pressure controller of tower top, and the top of the overhead condenser is provided with evacuated tube, described 2# regulating valves are in evacuated tube, and 2# regulating valves are connected with the pressure controller with by the Stress control 2# of rectifying column tower top The aperture of regulating valve.
5. cyclohexanol Mead-Bauer recovery system according to claim 4, it is characterised in that:The tower top temperature control unit bag Include the 3# regulating valves on condensing water conduit and be arranged at the 1# temperature controllers of tower top, and 3# regulating valves and 1# temperature controls Device is connected with by the aperture of the temperature control 3# regulating valves of rectifying column tower top.
6. cyclohexanol Mead-Bauer recovery system according to claim 4, it is characterised in that:Positioned at the cyclohexanol collection conduit It is provided with the cyclohexanol collection conduit after reflux line branch location on 4# regulating valves and flow indicator, the reflux line Provided with 5# regulating valves and 3# flow controllers, the rectifying column tower top is provided with 1# fluid level controllers, the backflow control unit bag Include the 4# regulating valves, flow indicator, 5# regulating valves, 3# flow controllers and 1# fluid level controllers, 4# regulating valves and 1# Fluid level controller is connected with by the aperture of the Liquid level 4# regulating valves of rectifying column tower top, 5# regulating valves and 3# flow controller phases The aperture of 5# regulating valves is even controlled with the flow in reflux line.
7. cyclohexanol Mead-Bauer recovery system according to claim 4, it is characterised in that:The control system also includes steam Flow controlling unit, the steam flow control unit includes the 8# regulating valves being located on jet chimney and located at rectifying column bottom 2# temperature controllers, and 8# regulating valves are connected with 2# temperature controllers with by the temperature control 8# regulating valves of rectifying column bottom Aperture.
8. cyclohexanol Mead-Bauer recovery system according to claim 4, it is characterised in that:The control system is also adopted including side Go out and 2# flow controllers are provided between control unit, described upper and lower two sections of packing section, the side extraction control unit includes institute State 2# flow controllers and located at side produce pipeline on 6# regulating valves, the 6# regulating valves be connected with 2# flow controllers with Flow between upper and lower two sections of packing section controls the aperture of 6# regulating valves.
9. cyclohexanol Mead-Bauer recovery system according to claim 4, it is characterised in that:The control system also includes restructuring Point collect control unit, the heavy constituent collect control unit include 7# regulating valves in the heavy constituent collection conduit and 2# fluid level controllers located at the rectifying column bottom, the 7# regulating valves are connected with by rectifying column bottom with 2# fluid level controllers Liquid level 7# regulating valves aperture.
10. cyclohexanol Mead-Bauer recovery system according to claim 1, it is characterised in that:The heavy constituent collection conduit is leaned on The position punishment of nearly rectifying column has installed decoking unit, and the decoking unit includes cyclohexanol recycling pipeline, the cyclohexanol One end of recycling pipeline is communicated in heavy constituent collection conduit, and the other end is communicated at the bottom of towe position of rectifying column, and hexamethylene Alcohol recycling pipeline is provided with flash tank, and the flash tank is connected between vavuum pump and flash tank and vavuum pump through pipeline and is provided with Vacuum breaker, the bottom of flash tank is through remaining heavy constituent pipeline communication to heavy constituent collection conduit;In cyclohexanol recycling pipe Between road and the communicating position and remaining restructuring subtube and the communicating position of heavy constituent collection conduit of heavy constituent collection conduit Provided with 4# stop valves.
CN201710535599.2A 2017-07-04 2017-07-04 A kind of cyclohexanol Mead-Bauer recovery system Pending CN107261540A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710535599.2A CN107261540A (en) 2017-07-04 2017-07-04 A kind of cyclohexanol Mead-Bauer recovery system

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710535599.2A CN107261540A (en) 2017-07-04 2017-07-04 A kind of cyclohexanol Mead-Bauer recovery system

Publications (1)

Publication Number Publication Date
CN107261540A true CN107261540A (en) 2017-10-20

Family

ID=60069798

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710535599.2A Pending CN107261540A (en) 2017-07-04 2017-07-04 A kind of cyclohexanol Mead-Bauer recovery system

Country Status (1)

Country Link
CN (1) CN107261540A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110141884A (en) * 2019-05-27 2019-08-20 中冶焦耐(大连)工程技术有限公司 The method and system of tower top regurgitant volume are controlled in tar production, benzene hydrogenation process
CN111494977A (en) * 2020-05-19 2020-08-07 上海盛剑环境系统科技股份有限公司 Stripping waste liquid recovery system and recovery method

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2241148Y (en) * 1994-08-30 1996-11-27 石家庄焦化厂 Compound tower for production of industrial naphthaline
CN1450033A (en) * 2002-04-10 2003-10-22 中国石油化工股份有限公司 Adiabatic flash method for styrene tar oil
CN1749227A (en) * 2005-10-19 2006-03-22 大连理工大学 Energ ysaving method for producing ethyl benzene by benzene and dry gas hydrocarbonization
CN1966428A (en) * 2006-10-16 2007-05-23 西安长庆科技工程有限责任公司 Gas field methanol sewage disposal process
CN101306973A (en) * 2007-05-16 2008-11-19 中国石油化工股份有限公司 Process for recovering ethylene in process of ethylene preparation by ethanol dehydration
CN202199146U (en) * 2011-09-13 2012-04-25 南京师范大学 External circular reaction side-discharge rectification apparatus in composite structure
CN103724192A (en) * 2013-09-05 2014-04-16 百川化工(如皋)有限公司 Energy-saving acetic ester refining method
CN105294604A (en) * 2014-07-24 2016-02-03 中国石油化工股份有限公司 Propylene oxide production device
CN206980148U (en) * 2017-07-04 2018-02-09 河南神马尼龙化工有限责任公司 A kind of cyclohexanol Mead-Bauer recovery system

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2241148Y (en) * 1994-08-30 1996-11-27 石家庄焦化厂 Compound tower for production of industrial naphthaline
CN1450033A (en) * 2002-04-10 2003-10-22 中国石油化工股份有限公司 Adiabatic flash method for styrene tar oil
CN1749227A (en) * 2005-10-19 2006-03-22 大连理工大学 Energ ysaving method for producing ethyl benzene by benzene and dry gas hydrocarbonization
CN1966428A (en) * 2006-10-16 2007-05-23 西安长庆科技工程有限责任公司 Gas field methanol sewage disposal process
CN101306973A (en) * 2007-05-16 2008-11-19 中国石油化工股份有限公司 Process for recovering ethylene in process of ethylene preparation by ethanol dehydration
CN202199146U (en) * 2011-09-13 2012-04-25 南京师范大学 External circular reaction side-discharge rectification apparatus in composite structure
CN103724192A (en) * 2013-09-05 2014-04-16 百川化工(如皋)有限公司 Energy-saving acetic ester refining method
CN105294604A (en) * 2014-07-24 2016-02-03 中国石油化工股份有限公司 Propylene oxide production device
CN206980148U (en) * 2017-07-04 2018-02-09 河南神马尼龙化工有限责任公司 A kind of cyclohexanol Mead-Bauer recovery system

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
臧福录: "《石油化工工艺工程师必读 第2册 多组分精馏的计算和分析》", 30 November 1998, 北京:中国石化出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110141884A (en) * 2019-05-27 2019-08-20 中冶焦耐(大连)工程技术有限公司 The method and system of tower top regurgitant volume are controlled in tar production, benzene hydrogenation process
CN111494977A (en) * 2020-05-19 2020-08-07 上海盛剑环境系统科技股份有限公司 Stripping waste liquid recovery system and recovery method
CN111494977B (en) * 2020-05-19 2023-08-25 上海盛剑环境系统科技股份有限公司 Stripping waste liquid recovery system and recovery method

Similar Documents

Publication Publication Date Title
CN100453137C (en) Alcohol quinque-towel differential pressure distilling arrangement and technique thereof
CN100378051C (en) Rectifying tech. and equipment of high purity methanol
CN101748037B (en) Special grade edible alcohol six-tower difference pressure distilling device and process thereof
CN203710716U (en) Device for improving recycling rate of alcohol ketone components in refining process of cyclohexanone
CN101874935A (en) Rectifying section tower bottom reboiling internal heat-integrated energy-saving rectifying apparatus and method
WO2021047393A1 (en) Rectification device and rectification method for oxo synthesis of acetic acid
CN106957214A (en) Methanol heat-pump distillation system and method
CN107261540A (en) A kind of cyclohexanol Mead-Bauer recovery system
CN105315132A (en) System and method used for energy utilization between ethylene glycol device dehydrating tower and refining tower
CN103420974A (en) Triformol refining system and method thereof
CN101412665B (en) Apparatus for coproduction of refined methanol and dimethyl ether or production of each of refined methanol and dimethyl ether from coarse methyl alcohol
CN201094869Y (en) Multipurpose internal reflux distillation device
CN206980148U (en) A kind of cyclohexanol Mead-Bauer recovery system
CN108525338A (en) Alcohol recycle rectifying device and alcohol recycle rectificating method
CN108530264A (en) New heat energy utilization system and heat energy utilization method in a kind of cyclohexanol production
CN110330418B (en) Method for recovering formaldehyde gas volatilized in normal pressure device in pentaerythritol production
CN213726490U (en) Pyridine recovery system for diosmin production
CN201567231U (en) Hydrogen chloride desorption tower device for recycling polycrystalline silicon production tail gas
CN208182895U (en) A kind of tetrahydrofuran fractional order reaction separator
CN109821267A (en) A kind of tetrahydrofuran recovery system
CN115140791A (en) Device and process for recovering and extracting furfural from process wastewater
CN204840984U (en) Rectifying device
CN210314061U (en) Rectification and purification device for synthesizing dimethyl oxalate by carbonylation of coal-made ethylene glycol
CN205227896U (en) Condensate water is recovery system again
CN101250257A (en) Polymerization esterification residual heat utilization method and apparatus

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right

Effective date of registration: 20180402

Address after: 467013 high tech Development Zone, Jianshe Road, Henan, Pingdingshan

Applicant after: HENAN SHENMA NYLON CHEMICAL Co.,Ltd.

Applicant after: PINGDINGSHAN PUEN TECHNOLOGY Co.,Ltd.

Applicant after: Henan Jiusheng Chemical Co.,Ltd.

Address before: 467013 high tech Development Zone, Jianshe Road, Henan, Pingdingshan

Applicant before: HENAN SHENMA NYLON CHEMICAL Co.,Ltd.

TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20191212

Address after: 467013 high tech Development Zone, Jianshe Road, Henan, Pingdingshan

Applicant after: HENAN SHENMA NYLON CHEMICAL Co.,Ltd.

Address before: 467013 high tech Development Zone, Jianshe Road, Henan, Pingdingshan

Applicant before: HENAN SHENMA NYLON CHEMICAL Co.,Ltd.

Applicant before: PINGDINGSHAN PUEN TECHNOLOGY Co.,Ltd.

Applicant before: Henan Jiusheng Chemical Co.,Ltd.

TA01 Transfer of patent application right
RJ01 Rejection of invention patent application after publication

Application publication date: 20171020

RJ01 Rejection of invention patent application after publication