CN106943775A - The device and method that solid liquid phase is continuously separated in caprolactam distillation weight raffinate - Google Patents
The device and method that solid liquid phase is continuously separated in caprolactam distillation weight raffinate Download PDFInfo
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- CN106943775A CN106943775A CN201710288480.XA CN201710288480A CN106943775A CN 106943775 A CN106943775 A CN 106943775A CN 201710288480 A CN201710288480 A CN 201710288480A CN 106943775 A CN106943775 A CN 106943775A
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- caprolactam
- clarified solution
- residue
- medial launder
- settler
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/003—Sedimentation tanks provided with a plurality of compartments separated by a partition wall
- B01D21/0033—Vertical, perforated partition walls
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/0039—Settling tanks provided with contact surfaces, e.g. baffles, particles
- B01D21/0045—Plurality of essentially parallel plates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/009—Heating or cooling mechanisms specially adapted for settling tanks
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- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the device and method that solid liquid phase in caprolactam distillation weight raffinate is continuously separated, the device includes settler, and its side is provided with charging aperture, and opposite side is provided with overfall, and bottom is provided with slag-drip opening；Overfall is connected with clarified solution medial launder, and slag-drip opening is connected with residue defecator；Clarified solution medial launder is connected to caprolactam process by pipeline and pump, and clarified solution medial launder is also connected with caprolactam technology waterpipe.It carries out cleaning dilution by using caprolactam technology water to clarified solution and residue, realizes caprolactam and continuously separating for oligomer and recycling for caprolactam technology water in caprolactam distillation weight raffinate.
Description
Technical field
The invention belongs to chemical technology field, it is related to the production of caprolactam, specially in caprolactam distillation weight raffinate
The device and method that solid liquid phase is continuously separated.
Background technology
Caprolactam distillation process is the final step of caprolactam refining.Oneself is reduced using high vacuum operation in distillation process
Lactams boiling point, can avoid caprolactam by high thermal polycondensation, while being added in distillation feeding liquid in alkali and that may be present few
Amount organic acid forms stable salt, to be separated in distillation with caprolactam, reduces the volatile base content of product.
But inevitably there is hot-spot situation, and be conducive to caprolactam again in steam-heated heater tubulation
The presence of the caustic soda and moisture of polymerization, so the polymerization of caprolactam can be caused, so that solid particle is formed, in order that these are poly-
The heavy constituents such as the caustic soda that the particle and early stage of compound formation are added can be excluded smoothly out of destilling tower, and destilling tower is carried out to evaporation capacity
Strict control, it is ensured that 1.5 ~ 2.0m of volume flow of vinasse3/ h, by analysis the raffinate solid concentration 0.8 ~
Between 3.0%wt, the change of its concentration is relevant with the control of the evaporation capacity of destilling tower.
Because 98% or so is all caprolactam in vinasse, it must reclaim, traditional way is that this is residual
Liquid is directly transmitted back to ammonium sulfate process with pump after being mixed with the condensed water of distillation process and the steam-to-vacuum pump of flash process and used,
Become extraction phase --- the crude oil of oneself extraction tower.This method does not pass through any processing, is simply followed in ammonium sulphate crystallizer and carrying
The circle of ring one, partial polymer can be discharged with ammonia sulfate crystal, and another part is then as crude oil enters oneself extraction tower.In short-term
Interior own extraction tower is also had no problem, and production is also compared normally, but as polymer is accumulated for a long time, own extraction tower operating mode meeting
There is larger fluctuation：One is extraction phase entrainment aqueous phase；Two be that raffinate aqueous phase amount is few, and own Cui Ta circle can not ensure, Er Qiecui
Substantial amounts of particulate matter is frequently accompanied by remaining aqueous phase, causes rotating disk and fixed disk to block.The fluctuation of extraction tower operating mode is to final production
Product yield and quality all cause larger fluctuation.
Many is also compared to the processing method of caprolactam vinasse in the same industry, respectively there is feature：
1）Batch distillation is carried out to vinasse：Multiple distillation stills are used, certain vinasse is put and enters, in high vacuum
It is lower caprolactam is evaporated after condense then to stop after impurity is more in kettle after recovery, a period of time again and cleared up, cleared up
Other kettle processing vinasse is used in journey.This method causes labor strength big, and intermittent operation is also unfavorable
It is stable in production；
2）Vinasse is sold：Improve the evaporation capacity of destilling tower as far as possible in the case of operating mode is suitable, reduce and steam
The flow of raffinate is evaporated, then plus other producer is sold to after little water and is purified.This method yield is low, and vinasse amount
Smaller solution causes raffinate pipeline easily to block, and regular causes distillation operating mode poor；
3）Intercepted using filter：Vinasse send ammonium sulfate process after being mixed with water, use filter, active carbon bed, filter
Cloth centrifuge etc., water-insoluble is filtered out.By using the sand core funnel G4 of different size：5-15μm、 G5：2-5μm 、
G6：<Weigh difference after the residual night filtration drying of 2 μm of counterweights, it is found that G4 weight is substantially smaller than G5 and G6, so water-insoluble
The diameter overwhelming majority of particle is below 5 μm, so common mechanical filter there is no great effect, and it is high-precision
Filter cloth centrifuge filter efficiency is again too low；
4）Physics is settled：Distillation weight raffinate is stored with storage tank, through standing after a while, makes granular water insoluble
Thing is deposited on tank bottom, and the liquid caprolactam of upper strata clarification is extracted to recycle, with the particle deposited in storage tank
Thing increases, and keeps apart storage tank after clarifying effect reduction, is come into operation again after eliminating particle thing after cleaning displacement.
Each caprolactam producer has the processing method of oneself to caprolactam vinasse, though its significant degree how
Sample, at least all assert that the polymer in caprolactam vinasse is harmful.
The content of the invention
, can it is an object of the invention to provide the device and method that solid liquid phase in a kind of caprolactam distillation weight raffinate is continuously separated
Realize caprolactam and oligomer in caprolactam distillation weight raffinate it is continuous separate and caprolactam technology water circulation profit
With.
In order to solve the above technical problems, the technical solution adopted in the present invention is：Solid-liquid in caprolactam distillation weight raffinate
The device mutually continuously separated, including settler, its side are provided with charging aperture, and opposite side is provided with overfall, and bottom is provided with slag-drip opening；
Overfall is connected with clarified solution medial launder, and slag-drip opening is connected with residue defecator；Clarified solution medial launder is connected by pipeline and pump
To caprolactam process, clarified solution medial launder is also connected with caprolactam technology waterpipe.
Further, described charging aperture is connected with caprolactam distillation weight raffinate pipeline, by being provided with valve at charging aperture
Door, is provided with branch pipe, it is connected to residue defecator between caprolactam distillation weight raffinate pipeline and valve.
Further, the settler is high-efficiency sedimentation device, is internally provided with internals, and top is provided with rupture pressure disc and individual calling
Valve, bottom is pyramidal structure, and settler is externally provided with heat tracing equipment；Settler is also associated with nitrogen pipeline.
It is preferred that scheme in, described internals are swash plate, perforated plate corrugated filler or wire packing, preferably metal slant board.
Further, the settler is connected using multiple, it is two neighboring between bottom is drawn by dividing plate
Point, the top of dividing plate is not contacted at the top of settler.
Further, the caprolactam technology waterpipe is also connected with flushing pipe, and it is located at slag-drip opening and clarified with residue
Between groove, and at slag-drip opening；Residue defecator is connected to caprolactam process by pipeline and pump.
Further, the bottom of the clarified solution medial launder sets Residue extraction pipeline, and it is connected to residue defecator, and its top is set
There is evacuated tube.
The invention further relates to the method that solid liquid phase is continuously separated in weight raffinate, bag are distilled to caprolactam using described device
Include following steps：
Caprolactam distillation weight raffinate is introduced into settler and settled, the temperature in control settlement device is at 70 ~ 90 DEG C, sedimentation
The stillness of night afterwards enters through overfall further to be settled in clarified solution medial launder, while by the technique in caprolactam technology waterpipe
Water is passed through clarified solution medial launder and the stillness of night therein is diluted, then the liquid in clarified solution medial launder is delivered into caprolactam
Process.
Further, the volume ratio of process water and the stillness of night are 1 ~ 5 in the clarified solution medial launder:1；In clarified solution medial launder
Liquid level in its total capacity 40 ~ 70%.
Further, when slag-drip opening carries out deslagging in settler, using the process water pair in caprolactam technology waterpipe
Pipeline between slag-drip opening and residue defecator is rinsed, and is clarified after flushing, and clarified solution is also delivered to caprolactam work
Sequence.
Solid content is 0.8 ~ 1.5 wt % in caprolactam distillation weight raffinate, and the device provided through the present invention and technique are carried out
Solids content is reduced to less than 0.1% in the clear liquid obtained after sedimentation clarification, and clear liquid is diluted with caprolactam technology water, it is to avoid high
The caprolactam solidification of concentration or the thermal loss with chuck pipeline and jacketed pump and heat tracing pipeline, the caprolactam of dilution
The aqueous solution directly sends the recycling of caprolactam process back to.
The solid phase of settler bottom is discharged into residue defecator by slag-drip opening after collecting and rushed using caprolactam technology water
The caprolactam washed in pipeline and dilution residue, the stillness of night can be with after residue defecator material is clarified through standing after a while
Send the utilization of caprolactam process back to, when solid phase is more in residue defecator, its solid phase is cleared up.
The separation of solid phase is not the final purpose of the invention in distillation weight raffinate.Inventor is residual by distillation weight in an experiment
Liquid mixed with water and benzene after find have obvious intermediate layer, this and in Caprolactam unit oneself extraction tower in intermediate layer very phase
Seemingly.Quiescent culture after the solid phase in distillation weight raffinate is mixed with the water and benzene of different proportion again is separated, is found intermediate layer " growing up "
For white particle, and its diameter can become big over time, and solid phase ratio is higher, and particle diameter is bigger, this and oneself
The cream-coloured coloured particles that extraction tower is excluded are the same, and simply the color of particle is different, that is, the polymer for distilling weight raffinate weight is own extraction
The arch-criminal that tower interphase and crystal are produced, it directly have impact on the operating condition of oneself extraction tower.
The present invention is by the way that by distillation weight raffinate, after preliminary separation, although oneself extracts, tower intermediate layer is also desultory to deposit
, but grain crystalline thing substantially disappears, then do not occurred, this makes entrainment phenomenon in oneself extraction tower benzene extraction phase substantially drop
It is low, removing of the impurity in oneself extraction tower is promoted, is had very great significance to the quality for improving product caprolactam.
Caprolactam destilling tower also has obvious change, the operation week of topmost destilling tower after oneself extraction tower operating mode changes
Phase extends.Caprolactam destilling tower will stop cleaning 2 ~ 4 times every month in the past, but after oneself extraction tower operating mode improves in oneself
The cycle of operation of acid amides destilling tower has averagely reached cleaning in 52 days once, and most long periods of time in order can reach 90 days.Caprolactam steams
Evaporate the tower cycle of operation extension also have one significantly change be exactly distill solid concentration in weight raffinate by original 1.8 ~
2.2%wt is reduced to 0.8 ~ 1.5%wt.
So the removing of solid phase is a benign circulation in caprolactam distillation weight raffinate, caprolactam is not only contributed to
The operation of device continuous-stable, also helps the lifting of product caprolactam quality.
Brief description of the drawings
Fig. 1 is the structural representation of apparatus of the present invention
Embodiment
The present invention is further illustrated with reference to embodiment, but the scope of protection of present invention is not limited to implement
The scope of example statement.
Embodiment 1：
As shown in figure 1, the present invention relates to the device that solid liquid phase in a kind of caprolactam distillation weight raffinate is continuously separated, including sedimentation
Device 1, its side is provided with charging aperture 11, and opposite side is provided with overfall 12, and bottom is provided with slag-drip opening 13；In the middle of overfall and clarified solution
Groove 2 is connected, and slag-drip opening 13 is connected with residue defecator 3；Clarified solution medial launder 2 is connected to caprolactam process by pipeline and pump
4, clarified solution medial launder 2 is also connected with caprolactam technology waterpipe 5.
Further, described charging aperture 11 is connected with caprolactam distillation weight raffinate pipeline 6, by being provided with charging aperture
Valve, is provided with branch pipe 7, it is connected to residue defecator 3 between caprolactam distillation weight raffinate pipeline 6 and valve.Due in oneself
Contain solid phase in acid amides distillation weight raffinate, pipeline solution is blocked, needed at interval of a period of time in cleaning, the present invention in cleaning
Using caprolactam technology water, contain solid phase in the process water after cleaning, it is clear to be directly discharged into the progress of residue defecator by branch pipe
Clearly, while avoiding process water from entering in settler, cause the polymerization of caprolactam, and form more solid particles.In addition, plus
The process water entered can be diluted to the caprolactam in residue defecator, be easy to the later stage to return sharp again in caprolactam process
With.
Further, the settler 1 is high-efficiency sedimentation device.It is internally provided with internals.Top is provided with rupture pressure disc and individual calling
Valve, to ensure equipment safety.Bottom is pyramidal structure, facilitates solid phase sedimentation collection.Settler is externally provided with heat tracing equipment, can be by
Caprolactam temperature control is at 70 ~ 90 DEG C, it is to avoid the caprolactam crystallization of high concentration.Settler is also associated with nitrogen pipeline 8, leads to
Nitrogen envelope is crossed, prevents that the caprolactam in settler from going bad with air contact, and the nitrogen pipeline is additionally provided with regulating valve, regulating valve
For direct-operated regulator.
Further, described internals are swash plate, perforated plate corrugated filler or wire packing, preferably metal slant board, it is to avoid stifled
Plug, convenient cleaning.
Further, the settler 1 is connected using multiple, it is two neighboring between bottom is drawn by dividing plate
Point, the top of dividing plate does not contact the top of settler 1.By the series connection of multiple settlers, clarifying effect is improved.
Further, the caprolactam technology waterpipe 5 is also connected with flushing pipe 9, and it is located at slag-drip opening 13 and residue
Between defecator 3, and at slag-drip opening 13；Residue defecator 3 is connected to caprolactam process 4 by pipeline and pump.Pass through
The setting can prevent the line clogging after deslagging；And the caprolactam in residue can be diluted by process water.
Further, the bottom of the clarified solution medial launder 2 sets Residue extraction pipeline, and it is connected to residue defecator 3, after sedimentation
Residue enter residue defecator；Evacuated tube is provided with the top of clarified solution medial launder, it is normal pressure groove.
Clarified solution discontinuous in residue defecator is transported to caprolactam process, is conveyed by pump, in the porch of pump
Solid concentration when reaching that 1%wt or run time reach 72h, the solid phase in residue defecator is cleared up；Residue defecator
For without top underground tank, easy cleaning solid residue.
Embodiment 2：Weight raffinate is distilled to caprolactam using said apparatus and carries out separation of solid and liquid, control caprolactam distillation
The evaporation capacity of tower, makes distillation weight raffinate flow reach 1.5m3/ h, analyzes its solid content for 0.8 ~ 1.2%wt, first draws weight raffinate
Enter in settler and settled, the temperature in control settlement device is at 70 ~ 75 DEG C, and the stillness of night after sedimentation enters clarified solution through overfall
Further settled in medial launder, while the process water in caprolactam technology waterpipe is passed through into clarified solution medial launder to therein
The stillness of night is diluted, then the liquid in clarified solution medial launder is delivered into caprolactam process.
In operating process, the volume ratio of process water and clear liquid is 1 ~ 5 in clarified solution medial launder:1, make caprolactam after mixing
The concentration of the aqueous solution is controlled in 20 ~ 50%wt, it is to avoid caprolactam crystallization or the fresh desalination of the too low supplement of concentration after excessive concentration
Water；Liquid level in clarified solution medial launder, 40 ~ 70%, avoids deslagging from making liquid level too low in its total capacity to allow some leeway
Or distill unrestrained liquid when raffinate amount is larger again.
In operating process, when slag-drip opening carries out deslagging in settler, using the process water in caprolactam technology waterpipe
Pipeline between slag-drip opening and residue defecator is rinsed, clarified after flushing, clarified solution is also delivered to caprolactam
Process.
By nearly bimestrial stable operation, the average value 0.09%wt of solid content in the clear liquid of subsider overflow, oneself extraction tower
Entraimnent does not occur for operating mode, and caprolactam destilling tower does not carry out parking cleaning.
Comparative example 1：
Certain 100kt/ Caprolactam unit, caprolactam distillation weight raffinate is directly transmitted back in oneself after being mixed with some processes water
Acid amides device reclaims caprolactam, but oneself extraction tower runs operating mode after a period of time and always easily fluctuated, and extraction phase has folder
Contain substantial amounts of particulate matter in band, raffinate phase, be very easy to block rotating disc column and pipeline, be accomplished by within about 4 months or so parking pair
Oneself is cleared up extraction tower.The cycle of operation of caprolactam destilling tower also substantially shortens during oneself extraction tower fluctuation of operating conditions in addition, oneself
The wire mesh demister upper and lower temperature difference increase of lactams destilling tower, does not reach and adhere on output demand, parking checking wire mesh demister
The powdered substance of a large amount of whites, makes the increase of wire mesh demister pressure difference, in the case where ensureing yield, destilling tower about 7 days will
A parking wire mesh demister of cleaning.In order to solve the problems, such as the caprolactam destilling tower cycle of operation, at that time directly by caprolactam
Distillation weight raffinate sale a part, it is evident that caprolactam destilling tower the cycle of operation increase, oneself extraction tower operating mode also have inclination
Turn.
Comparative example 2：
With same 100kt/ Caprolactam units in comparative example 1, a 200m is added3Storage tank as subsider to oneself
Clarified caprolactam is reclaimed after particulate matter sedimentation in lactams weight raffinate, the caprolactam solid content of clarification is reduced to
0.3% or so, but the solid content after sedimentation after a while in clarified solution can gradually increase, so as to influence caprolactam
The destilling tower cycle of operation and own extraction tower operating mode, this is accomplished by regularly clearing up storage tank, and labor intensity is too big.
Compared with comparative example 1 and 2, using in the distillation of same 100kt/ Caprolactam units generation in embodiment 2
Raffinate, after implementing according to apparatus of the present invention and method, is grasped by the deslagging for continuously clarifying caprolactam vinasse and discontinuity
Make, clarification caprolactam solid content is stable, and the caprolactam destilling tower cycle of operation reaches 60 days or so below 0.1%, and oneself extracts tower
Also continuous operation reaches more than 480 days, does not substantially produce influence to the caprolactam destilling tower cycle of operation and oneself extraction tower operating mode.
Claims (10)
1. the device that solid liquid phase is continuously separated in caprolactam distillation weight raffinate, it is characterised in that：Including settler（1）, one
Side is provided with charging aperture（11）, opposite side is provided with overfall（12）, bottom is provided with slag-drip opening（13）；Overfall and clarified solution medial launder
（2）Connection, slag-drip opening（13）With residue defecator（3）Connection；Clarified solution medial launder（2）Acyl in oneself is connected to by pipeline and pump
Amine process（4）, clarified solution medial launder（2）It is also connected with caprolactam technology waterpipe（5）.
2. device according to claim 1, it is characterised in that：Described charging aperture（11）With caprolactam distillation weight raffinate
Pipeline（6）Connection, by being provided with valve, caprolactam distillation weight raffinate pipeline at charging aperture（6）Branch pipe is provided between valve
（7）, it is connected to residue defecator（3）.
3. device according to claim 1, it is characterised in that：The settler（1）For high-efficiency sedimentation device, it is internally provided with
Internals, top is provided with rupture pressure disc and single breathing valve, and bottom is pyramidal structure, and settler is externally provided with heat tracing equipment；Settler is also connected with
There is nitrogen pipeline（8）.
4. device according to claim 3, it is characterised in that：Described internals are swash plate, perforated plate corrugated filler or silk screen
Filler, preferably metal slant board.
5. device according to claim 1, it is characterised in that：The settler（1）Connected using multiple, adjacent two
Bottom is divided by dividing plate between individual, the top of dividing plate does not contact settler（1）Top.
6. device according to claim 1, it is characterised in that：The caprolactam technology waterpipe（5）It is also connected with rinsing
Pipeline（9）, it is located at slag-drip opening（13）With residue defecator（3）Between, and close to slag-drip opening（13）Place；Residue defecator（3）
Caprolactam process is connected to by pipeline and pump（4）.
7. device according to claim 1, it is characterised in that：The clarified solution medial launder（2）Bottom set Residue extraction pipeline,
It is connected to residue defecator（3）, its top is provided with evacuated tube.
8. the side that solid liquid phase is continuously separated in weight raffinate is distilled to caprolactam using claim 1-7 any one described device
Method, it is characterised in that comprise the following steps：
Caprolactam distillation weight raffinate is introduced into settler and settled, the temperature in control settlement device is at 70 ~ 90 DEG C, sedimentation
The stillness of night afterwards enters through overfall further to be settled in clarified solution medial launder, while by the technique in caprolactam technology waterpipe
Water is passed through clarified solution medial launder and the stillness of night therein is diluted, then the liquid in clarified solution medial launder is delivered into caprolactam
Process.
9. method according to claim 8, it is characterised in that：The volume of process water and the stillness of night in the clarified solution medial launder
Than for 1 ~ 5:1；Liquid level in clarified solution medial launder is in its total capacity 40 ~ 70%.
10. method according to claim 8, it is characterised in that：When slag-drip opening carries out deslagging in settler, using acyl in oneself
Process water in amine technique waterpipe is rinsed to the pipeline between slag-drip opening and residue defecator, is clarified after flushing,
Clarified solution is also delivered to caprolactam process.
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| CN201710288480.XA CN106943775B (en) | 2017-04-27 | 2017-04-27 | Device and method for continuously separating solid phase from liquid phase in caprolactam distillation heavy residual liquid |
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| CN109173673A (en) * | 2018-10-25 | 2019-01-11 | 山东环达环保科技有限公司 | Tar slag-drip opening slag-draining device and exhaust gas treating method and device |
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| CN115738477A (en) * | 2022-11-17 | 2023-03-07 | 科城精铜(广州)有限公司 | Copper rod rolling emulsion circulating system and method |
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| CN109173673A (en) * | 2018-10-25 | 2019-01-11 | 山东环达环保科技有限公司 | Tar slag-drip opening slag-draining device and exhaust gas treating method and device |
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| CN115738477A (en) * | 2022-11-17 | 2023-03-07 | 科城精铜(广州)有限公司 | Copper rod rolling emulsion circulating system and method |
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| CN106943775B (en) | 2020-02-14 |
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