CN207313271U - MTO washes the hydraulic art continuous cycle of operation extended device - Google Patents

MTO washes the hydraulic art continuous cycle of operation extended device Download PDF

Info

Publication number
CN207313271U
CN207313271U CN201721093388.XU CN201721093388U CN207313271U CN 207313271 U CN207313271 U CN 207313271U CN 201721093388 U CN201721093388 U CN 201721093388U CN 207313271 U CN207313271 U CN 207313271U
Authority
CN
China
Prior art keywords
water
oil
particle
mto
washing water
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.)
Active
Application number
CN201721093388.XU
Other languages
Chinese (zh)
Inventor
陈建琦
时代
吕文杰
李剑平
黄渊
汪华林
钱柯伟
李军
潘风光
徐芸
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.)
Zhejiang Xing Xing New Energy Technology Co Ltd
East China University of Science and Technology
Original Assignee
Zhejiang Xing Xing New Energy Technology Co Ltd
East China University of Science and Technology
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 Zhejiang Xing Xing New Energy Technology Co Ltd, East China University of Science and Technology filed Critical Zhejiang Xing Xing New Energy Technology Co Ltd
Priority to CN201721093388.XU priority Critical patent/CN207313271U/en
Application granted granted Critical
Publication of CN207313271U publication Critical patent/CN207313271U/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Catalysts (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

This disclosure relates to MTO washes the hydraulic art continuous cycle of operation extended device, there is provided MTO washes the hydraulic art continuous cycle of operation extended device, which includes:Mini-hydrocyclone separation device (5), for MTO washing waters to be carried out micro- eddy flow processing, to remove the free oil in water removal;The ebullated bed separator (7) being connected with mini-hydrocyclone separation device (5), for handling the washing water after micro- cyclone deoiling, to remove oil emulsion, dispersed oil and catalyst fines.

Description

MTO washes the hydraulic art continuous cycle of operation extended device
Technical field
The disclosure belongs to chemical industry environmental protection field, is related to a kind of using mini-hydrocyclone separation device and ebullated bed separator long period fortune Row removes the method and apparatus of grease and catalyst granules in MTO technology washing water, is particularly suitable for separation equipment Continual and steady operation, reduces the later stage clean and maintenance of relevant device.Specifically, disclosure combination cyclonic separation and grain bed Separation and backwashing technology, there is provided the combination separation method and device of a kind of methanol-to-olefins washing water long-term operation.
Background technology
Methanol-to-olefins, abbreviation MTO (Methanol to Olefins) refer to using methanol as raw material, anti-by being catalyzed The process of low-carbon alkene should be prepared.The reaction generally realizes that used catalyst is mostly 200nm~20 by fluidized-bed reactor μm SAPO-34 molecular sieves.Catalyst powder is last is sent to urgency through three-stage cyclone separator recycling for high-temperature product gas in reactor Cold tower, gas are washed to leading to water scrubber after 109 DEG C or so through chilling tower cooler, sent again after washing to separation of olefins unit.By The limitation of cyclone separator separation accuracy, fine catalyst powder of the part particle diameter less than 10 μm are sent to chilling tower with product gas. Meanwhile there are the organic oxygen-containing compounds such as unreacted methanol, dimethyl ether and the intermediate product oil wax material reacted on a small quantity (more than 90% is aromatic hydrocarbons) can together enter chilling tower and water scrubber with reaction gas.Since chilling tower operation temperature is higher, and produce Product gas and chilled water (chw) time of contact are short, therefore chilling tower can wash most of catalyst fines, and organic oxygen-containing chemical combination Thing and oily wax largely enter in washing water.Since reaction process can produce a certain amount of water, what usual water scrubber condensed out Waste water is to contain the organic oxygen-containing such as 0.5 μm~20 μm of SAPO-34 molecular sieve catalysts powder and a small amount of methanol, dimethyl ether The hot waste water (85~95 DEG C) of compound and the oily wax material (oil content is 200~700mg/L) based on aromatic hydrocarbons.
In actual production, washing water oil content, sets oil partition tank in water scrubber in order to control, will be floated by Liquid level in water Oil is interposed between discharge water scrubber in oil partition tank.However, in actual operation, due to washing water after oil removal oil content still have 150~ 300mg/L causes low-temperature space wax deposition in washing water circulation system serious, and washing water- to-water heat exchanger, air cooler and washing tower tray floor block Seriously, the long-period stable operation of device has been seriously affected, and has caused heat-exchange system heat exchange efficiency low, has needed frequent clean.Together When, since the oil in washing water is there are certain emulsification, cause degreaser cyclone to be not thorough oily wax removing in water;And due to Gatch is more in water, while still suffers from the catalyst fines of small particle, easily causes washing water filter element of precision filter to block, Equipment can not normal operation.In addition catalyst particles enter in stripping tower the stable operation that can also influence stripping tower, therefore find Efficient separation de-oiling de-solid method is particularly significant.
At present, common de- solid de-oiling method mainly has sedimentation, centrifugal separation, electrostatic separation method and membrane separation process Deng with the rise of fine slurry process demand in the industry in recent years, membrane separation technique obtains extensive concern.But due to methanol alkene The features such as often presence processing flow is big in the industrial environments such as hydrocarbon, solid holdup and high oil content, the secondary filter technology such as UF membrane In the presence of it is easy block, maintenance cost is big and of high cost the shortcomings of.
Solid oil removing process is taken off for MTO washing waters, Chinese patent application CN104649446A proposes more using more than three Runner rotating valve is in parallel to carry out MTO washing waters and chilled water (chw) separation of solid and liquid to be separated by filtration unit, but more according to its experiment description For more than 3 μm of catalyst granules of processing particle diameter, good removal effect can not be played to less than 3 μm catalyst granules.And Rotary valve is cheap as one, widely used mechanical equipment, mainly has feed, dedusting, discharging etc. should in the world at present With, do not possess substantially to washing water carry out oil removal treatment function.
Chinese patent application CN103951098A proposes to carry out isolation of purified to washing water using ultrafiltration membrane, and combines three-phase Separator recycles catalyst.This application make use of relatively advanced membrane separation technique to handle washing water and recycle catalysis Agent particle is to increase economic efficiency.But film footpath used in display is 5~200nm in this application, and the processing to subparticle is more smart Carefully, but in the very high washing water treatment procedure of the oil content of big flow easily pressure difference is caused to raise, treatment effeciency reduces.And its Filter element is the series connection of filter membrane, and in recoil since dope solid holdup and oil content are very high, the filter membrane of series connection increases pressure difference Rise progressively, be unfavorable for big flow processing procedure steady and continuous operation.
Chinese patent application CN102093153A and CN101352621A propose using micro- cyclone technique to MTO chilled water (chw)s into Row mini-hydrocyclone separation, to remove the catalyst granules wherein carried secretly.Mini-hydrocyclone separation utensil has the applicability wide, cheap, easy The advantages that safeguarding, contrast separation accuracy are 5-10 μm of common cyclone separator separative efficiency higher, but fine to less than 3 μm Fines below particle, especially 1 μm there are separative efficiency it is limited the problem of, and due to its design feature easily cause it is stifled The problems such as plug, high pressure drop, increase energy consumption output and the cleaning and maintenance difficulty in later stage.In addition containing a large amount of organic in washing water Oxygenatedchemicals and oily wax, micro- eddy flow is limited to the separating effect of oil, and the grease and fines in waste water are to follow-up vapour Carry in process and bring irregular operation factor.
In conclusion it is not thorough easily blocking, equipment for the existing separation of current methanol-to-olefins washing water circulation system The problem of frequent clean, short continuous cycle of operation, need to improve a kind of new side of continuous operation to the efficiently de- solid oil removing of washing water Method and device.
Utility model content
Present disclose provides a kind of MTO to wash the hydraulic art continuous cycle of operation extended method and device, has reached efficient Washing water oil content, solid content are reduced, while extends the purpose of equipment stable operation cycle.This method and device are easy and effective, Solve that filter plant present in existing process easily blocks, frequent clean, continuous operating time are short and oily wax and solid in water Particulate matter removes halfway technological deficiency.
On the one hand, present disclose provides a kind of MTO to wash the hydraulic art continuous cycle of operation extended method, and this method includes Following steps:
(i) MTO washing waters are subjected to micro- eddy flow processing, to remove the free oil in water removal;And
(ii) washing water after micro- cyclone deoiling is sent into ebullated bed separator to be handled, to remove oil emulsion, divide Dissipate oil and catalyst fines;
Wherein, after the continuous operation of ebullated bed separator is accumulate to certain value to operation pressure difference, washing water backwashing is passed through, Nitrogen mix backwash can be added, particle layers is fluidised to boiling-like completely;
Backwash flow is adjusted, the catalyst fines intercepted with release, empties hole pollutant holding capability;
Gas-liquid-solid mixture through backwash is subjected to three phase separation, the filtrate of gained is back to particle layers, and entrainment is urged The counter-flushing liquid and backwash gas of agent are outer respectively to be arranged;And
After backwash, normal operating conditions is switched to, grain bed completes active regeneration, and equipment continues to run with.
In one preferred embodiment, this method further includes:(iii) washing water that will be handled through ebullated bed separator Carry out stripping processing.
In another preferred embodiment, the operating temperatures of the MTO washing waters is 85 DEG C or higher, solid catalysis The content of agent particle is 0.1~1.0g/L, and the average grain diameter of solid catalyst particle is 0.5~5 μm, the oil content in washing water For 200~700mg/L.
It is aqueous in oil phase in washing water after being handled through ebullated bed separator in another preferred embodiment Amount is down to less than 10%, and oil content is down to below 30mg/L, and solid suspension content is down to below 20mg/L.
The use of medium is the polymorphic shape that particle diameter is 0.2mm~3mm in grain bed in another preferred embodiment Granule filter material, wherein ball-type rate is lower, particle diameter is smaller, and dirty rate of receiving is higher;Ball-type rate is higher, particle diameter is bigger, rotation regeneration efficiency It is higher.
In another preferred embodiment, washing water stoste enters from ebullated bed separator bottom drives particle layers Boiling, backwash flow velocity is 10~20m/h;First gravitational settling after dope is discharged is backwashed, then carries out bottom aqueous waste material Dehydration, to recycle.
On the other hand, present disclose provides a kind of MTO to wash the hydraulic art continuous cycle of operation extended device, the device bag Include:
Mini-hydrocyclone separation device, for MTO washing waters to be carried out micro- eddy flow processing, to remove the free oil in water removal;
The ebullated bed separator being connected with mini-hydrocyclone separation device, for handling the washing water after micro- cyclone deoiling, to go Except oil emulsion, dispersed oil and catalyst fines.
In another preferred embodiment, which further includes:
The settling tank being connected with mini-hydrocyclone separation device, the washing water for being discharged to mini-hydrocyclone separation device settle, real Existing water-oil separating;
The surge tank being connected with ebullated bed separator, for storing through the purified washing water of ebullated bed separator;
With buffering tank connected stripping tower, the washing water for will be handled through ebullated bed separator carries out stripping processing.
In another preferred embodiment, the ebullated bed separator is the combination of three phase separator and grain bed, Medium used is more size Multiple Shape tandem compounds of granule filter material.
In another preferred embodiment, the particle selected in the grain bed medium, the change of its particle size slope 50% or higher after, increase with particle rotation intensity under flow, rotation turn up 1500rad/s or higher, particle layers regeneration Efficiency improves.
Beneficial effect:
The utility model using the method and apparatus that mini-hydrocyclone separation device and ebullated bed separator combine to MTO washing waters into The de- solid oil removal treatment of row, realizes that granules regeneration is reset with pollutant holding capability with reference to backwash design;Preferably reaching reduces in washing water Oil content is to below 50mg/L, solid holdup to below 50mg/L, requirement of the dust residual rate below 5% after backwash;Realize Removal efficiency is high, the cycle of operation is long, the requirement easy to safeguard and operated easy to upstream device stabilization.
Brief description of the drawings
Attached drawing is provided for further understanding to the utility model, it simply form the part of this specification with The utility model is explained further, does not form the limitation to the utility model.
Fig. 1 be according to the MTO of an embodiment of the disclosure wash the hydraulic art continuous cycle of operation extended method and The process flow diagram of device.
Fig. 2 is to wash the hydraulic art continuous cycle of operation extended method according to the MTO of the another embodiment of the disclosure With the process flow diagram of device.
Fig. 3 is the traffic monitoring figure continuously run using backwash maintenance equipment small-scale experiment.
Principle schematic when Fig. 4 is the backwash of ebullated bed separator.
Embodiment
For present inventor by extensive and found after in-depth study, operation flow this kind of to MTO washing waters is big, contains Oil cut rate is high, solid content is relatively low and small the easy of (being usually 1-10 μm) of entrained catalyst subparticle particle diameter blocks difficult stable operation System for handling, mini-hydrocyclone separation are that a kind of cheap economic, easy to use, applicability is wide and the effective method of processing;Compare In common cyclone, international level at present, it generally can remove more than 6 μm of fine catalyst particles, but for less than 5 μm Fines removal efficiency it is more general;Mini-hydrocyclone separation device is strengthened by parallel connection, its separative efficiency can be much higher than commonly Cyclone, separates and recovers less than 5 μm particles;But since washing water oil content is high, oil is relatively viscous, and there is attachment is micro- rotation Stream separator inner wall separates bad situation, and entrained catalyst particles are mostly 1~10 μm in washing water, wherein less than 3 μm are urged Agent content is not high, but puts into practice 3 discoveries by industrial experiment, and the blocking of separator is often accelerated in the entrainment of superfine catalyst, The cleaning frequency of device is added, and is unfavorable for recycling recycling for waste water, therefore has inspired exploitation deep layer Bed Filtration Device carries out separating treatment to fines in washing water and oil.
The technical concept of the utility model is as follows:
Pre-separation is carried out to MTO washing waters by mini-hydrocyclone separation device;Washing water after separation travels further into boiling Bed separator carries out in-depth filtration;Washing water after oil removing and filtering enters in surge tank, to be recycled or be stripped Processing;Wherein, after the continuous operation of ebullated bed separator is accumulate to certain value to operation pressure difference, it is passed through from ebullated bed separator outlet Washing raw water, which carries out backwash, makes particle media be in boiling-like, and medium occurs high speed rotation and mutually collision, realizes interceptor Release and the regeneration of media filtration activity, lift the pollutant holding capability of ebullated bed separator, so as to greatly reduce the blocking of equipment again And clean and maintenance, washing water decontamination process continue stable operation repeatedly.
In the first aspect of the disclosure, there is provided a kind of MTO washes the hydraulic art continuous cycle of operation extended method, the party Method includes:
The washing water of the reaction gases such as oil phase thing and methanol such as catalyst granules, the aromatic hydrocarbons such as entrainment SAPO-34 passes through centrifugal pump Extracted out from water scrubber bottom, pre-separation oil removing is carried out by mini-hydrocyclone separation device first, go to water removal middle reaches from oil;
The rich oil waste water that degreaser cyclone is isolated is sent to settling tank, further separates the grease phase in oil phase, oil phase For freshening processing;
Washing water after cyclone deoiling is discharged through the underflow of mini-hydrocyclone separation device, and the waste water isolated in settling tank is together Boiling bed filter is passed through, remaining difficult separation capillary oil in water is filtered out using effects such as interception, the absorption for separating medium particle (oil emulsion, dispersed oil) etc., while filter the superfine catalyst powder in washing water;
Wherein, after grain bed pressure difference is accumulate to certain value, backwashing state is switched to, by the washing water after cyclone deoiling Reversely together it is passed through by the former outlet mixing nitrogen of boiling bed filter and filtrate in bed is backwashed, it is in boiling-like to make filtrate State;
Adjust recoil flow so that the abundant rotation of filtrate and collision, discharge duct adsorption space, and accelerate to intercept between filtrate The removing of thing and surface contaminant;
By the hierarchical composition of different filtrate media, particle rotating speed is set to maintain more than 1500rad/s, ball-type rate is low, grain Scope wide media mix in footpath can improve rotating speed within the specific limits, accelerate regeneration;
After the gas-liquid-solid mixture of backwash is by three phase separator, filtrate is back to bed, the recoil of entrained catalyst Washing lotion and backwash gas outside top liquid phase, gaseous phase outlet respectively by discharging;
After backwashing a period of time, work filtration condition is switched to, recoil floss hole is closed.
It is preferred that recoil flow is adjusted to 50~90m3/h。
It is preferred that backwash when increase flow, make particle media liquid stream drive issue be born from turn and collision, accelerate surface And in duct pollutant removing, the dope of backwash from the liquid-phase outlet discharge of three phase separator at the top of granular bed filters, Processing recycling can be carried out to bottom dope by dehydration techniques such as centrifugal dryings after gravitational settling.
It is preferred that interior when 8 is small before continuous operation, pressure difference rise is slow and is less than 0.1MPa;1 is recoiled when often operation 10 is small It is secondary, realize filtrate active regeneration, after recoil the change of operating flux pressure difference with it is initial consistent.
It is preferred that during oil removing takes off admittedly, the washing water after oil removing and filtering is temporarily stored in surge tank, part warp Return to water scrubber after cooling to recycle, a part is sent to stripping tower and carries out stripping processing, isolates purified water and oil phase.
It is preferred that the purification method, which includes mini-hydrocyclone separation, Bed Filtration and follow-up stripping tower, handles three kinds points From the series combination of mode.
It is preferred that the operating temperature of the washing water is 85~95 DEG C, solid particle is methanol-to-olefin catalyst particle Fine powder, is usually SAPO-34 molecular sieve powders, solid content 0.1-0.5g/L, average grain diameter is 0.5~5 μm.
It is preferred that the isolation of purified is made of mini-hydrocyclone separation and the separation of deep layer grain bed, wherein mini-hydrocyclone separation can Initial gross separation larger particles, grain bed are separated except the oily wax component such as fines and aromatic hydrocarbons.
It is preferred that the washing water treating capacity is 35~65m3/ h, recoil flow velocity realize 1500rad/s up to 10~20m/s Particle rotation above, completes seed activity regeneration.
It is preferred that the backwash effect is good, initial backwash liquor solid concentration is down to after backwash 1min up to 3.2% 287mg/L, filter material surface catalyst residual rate effectively realizes regeneration below 5% after backwash.
It is preferred that washing water oil content is 200~700mg/L, net by cyclone deoiling and the combination of deep layer mechanical filter After change, oil content is down to below 50mg/L in water, and solid suspension content is down to below 50mg/L.
In the second aspect of the disclosure, there is provided a kind of MTO washes the hydraulic art continuous cycle of operation extended device, the dress Put including:
Mini-hydrocyclone separation device, for carrying out pre-separation to the larger catalyst granules carried secretly in chilled water (chw);Settling tank, is used for Handle the rich oil waste water after the separation of micro- cyclone;Deep layer granular bed filters, for the washing water after micro- cyclone into Row secondary purification, can be connected with dehydration devices such as nitrogen inlet, settling tank, surge tank and drying machines;Three phase separator, for pair The separation and recovery of dope and solid filtrate when deep layer granular bed filters backwash;Surge tank, water filtered fluid is washed for storing, Device is set to be in continuous and steady operation state;Stripper, for the washing after mini-hydrocyclone separation and deep layer Bed Filtration Water carries out stripping processing.
It is preferred that the separator is by micro- spiral-flow filter and ebullated bed separator (three phase separator and deep layer grain bed Filter) it is composed in series.
It is preferred that the pressure loss of micro- spiral-flow filter is 0.15-0.30MPa, the pressure damage of deep layer granular bed filters Lose as 0.01-0.30MPa.
It is preferred that the medium of the deep layer granular bed filters is quartz sand, anthracite, fruit of the particle diameter in 0.2mm~3mm The tandem compound of more size Multiple Shapes of the granule filter materials such as shell, activated carbon and carbon ball, for example, using the smokeless coal particles of 1-2mm With the tandem compound of 0.5-1.0mm quartz sand particles, 1-2mm quartz sand particles, 0.5-1.0 carbon balls particle and 0.3-0.5mm stones Tandem compound of sand particle etc..
Below referring to attached drawing.
Fig. 1 be according to the MTO of an embodiment of the disclosure wash the hydraulic art continuous cycle of operation extended method and The process flow diagram of device, solid content relatively low operating mode higher suitable for oil content.As shown in Figure 1, methanol is sent into reaction After being reacted in device 1, MTO reaction gases are discharged from 1 top exit of reactor, and entrained catalyst particles etc., which enter in chilling tower 3, reacts It is sent into water scrubber 4 and washes afterwards, the reaction gas of Removal of catalyst goes out water scrubber from top, separates alkene;Unreacted catalyst Feeding catalyst regeneration tower 2 is discharged by 1 outlet at bottom of reactor to regenerate, the gas (CO of gained2Deng) by 2 top exit of regenerator Discharge, regenerated catalyst discharge Returning reactor 1 by 2 outlet at bottom of regenerator;Water and the catalyst fines that wash out are from water Wash bottom of towe discharge, i.e. washing water;Washing water is sent to mini-hydrocyclone separation device 5 by centrifugation pumped, a large amount of washing waters for carrying grease secretly Discharged from overflow port, be sent to settling tank 6 and settled, realize water-oil separating, and together carry out with the oil from stripper 10 Dirty oil recycling;The washing water of a large amount of entrained catalysts is discharged from underflow opening, is sent to ebullated bed separator 7 and is carried out secondary purification; First it is temporarily stored in surge tank 8 through the purified washing water of grain bed deep layer, a part and the washing after settling tank separates oil Water is together sent to stripping tower 10 and carries out stripping processing, and a part is sent to water scrubber 4 and carries out circulation profit after the cooling of cooler 9 With;The purification Water Sproading that stripper 10 obtains;Period surge tank level stability is more than 1/2, to be maintained when device backwashes Stable operation;After pressure difference rises to certain value, recoil state is switched to, mini-hydrocyclone separation device underflow washing water is separated from ebullated bed The former outlet of device, together by bottom input, makes particle in the rotation of boiling-like component and collides realization regeneration, recoil dope with nitrogen Discharged from the three phase separator liquid-phase outlet on ebullated bed separator top, be sent to settling tank 6 and separated;Recoil finishes, particle Bed media regeneration is completed, and micro- cyclone underflow washing water is inputted by 7 upper inlet of ebullated bed separator again, switches to normal work State.
Fig. 2 is to wash the hydraulic art continuous cycle of operation extended method according to the MTO of the another embodiment of the disclosure It is relatively low suitable for oil content with the process flow diagram of device, the higher operating mode of solid content.It is different from flow shown in Fig. 1 It is that the sedimentation water after mini-hydrocyclone separation also carries out second particle bed purification, using what is recycled as another strand of return water scrubber Waste water;Ebullated bed dope is individually handled during backwash, is not sent to settling tank;Sample tap is set in surge tank water outlet, works as water sample Meet during conditions of discharge (petroleum substance≤20mg/L, COD≤1200mg/L, BOD≤5500mg/L), can be straight without stripping tower Run in and put.
Flow with respect to Fig. 1, the flow of Fig. 2 individually handle recoil dope, can pass through sedimentation, centrifuge or dry de- The series of process such as water, complete the purification of waste liquid and the recycling of catalyst;Its effluent is more environmentally protective;Work as at the same time Water sample can directly carry out sewage method when qualified, greatly reduce the spending using stripping tower and energy consumption.
As shown in Fig. 2, methanol is sent into reactor 1 after reacting, MTO reaction gases are discharged from 1 top exit of reactor, reaction Gas and entrained particles, which enter to be sent into water scrubber 4 after reaction in chilling tower 3, washes, and unreacted catalyst is by 1 bottom of reactor Outlet discharge is sent into catalyst regeneration tower 2 and is regenerated, the gas (CO of gained2Deng) by the discharge of 2 top exit of regenerator, it is regenerated to urge Agent discharges Returning reactor 1 by 2 outlet at bottom of regenerator;Alkene etc. discharges separation and recovery above water scrubber 4, is washed in tower Water is sent to mini-hydrocyclone separation device 5 by centrifugation pumped, and rich oil is discharged from overflow port, is sent to settling tank 6 and is settled to realize Dirty oil recycling, wash water containing solid water are discharged from underflow opening, and water is mutually together sent to the progress two level of ebullated bed separator 7 in settling tank Purification;It is temporarily stored in together in surge tank 8 through the purified washing water of grain bed deep layer and sedimentation water, a part is returned through cooler 9 Return water scrubber 4 to circulate, a part is sent to stripping tower 10 and carries out stripping processing;The Water Sproading that stripper 10 obtains, obtained oil With the oily together degreaser freshening from settling tank 6;Surge tank liquid level keeps more than 1/2 so that during backwash, recirculated water and place Reason process can be normally carried out;After pressure difference rises to certain value, recoil state is switched to, recoil dope is from ebullated bed separator top Three phase separator liquid-phase outlet discharge, settled, the series of process such as pressure-filtering dehydration drying, obtains urging for recoverable Agent;Recoil finishes, and grain bed media regeneration is completed, and mini-hydrocyclone separation device underflow washing water is again by above ebullated bed separator Entrance inputs, and switches to normal operating conditions;When water sample sampling meets standard outside surge tank (petroleum substance≤20mg/L, COD≤1200mg/L, BOD≤5500mg/L), can directly outer it arrange, it is not necessary to stripper processing.
Fig. 3 is the traffic monitoring figure continuously run using backwash maintenance equipment small-scale experiment.Fig. 3 is shown according to this reality The changes in flow rate of pilot plant test more than continuous and steady operation 60h is realized by backwashing with new ebullated bed separator.Such as Interior when 8 is small before continuous operation shown in Fig. 3, pressure difference rise is slow, pressure difference < 0.1MPa, and after being backwashed, medium activity is realized High-lighting regenerates, and stable continuous operation can be realized on the basis of ensureing to efficiently separate.
Principle schematic when Fig. 4 is the backwash of ebullated bed separator.As shown in figure 4, rotation occurs for bed endoparticle with touching Hit, realize the removing of pollutant and the duct regeneration of medium.
Embodiment
The utility model is expanded on further with reference to specific embodiment.It should be appreciated, however, that these embodiments are only used In explanation the utility model without forming the limitation to the scope of the utility model.The examination of actual conditions is not specified in the following example Proved recipe method, usually according to normal condition, or according to the condition proposed by manufacturer.Unless otherwise indicated, all percentage With number by weight.
Embodiment 1:
1. implement overview
During 1,800,000 tons/year of MTO technologies, according to the method for the utility model, using ebullated bed Purifier, to be purified to the washing water containing solid catalyst and oil, realizes the removing of dead catalyst particulate, mesh It is preceding to have completed lab scale and pilot experiment.
2. material properties and relevant parameter
Methanol-to-olefins washing water is liquid-solid two-phase mixture, contains solid catalyst particle and oil in water;At washing water Reason amount is 35~65m3/ h, operation temperature are 90 DEG C, and dead catalyst content is 0.1~0.5g/L, and average grain diameter is 2.0 μm, oil Nearly 200~the 700mg/L of content.
3. ebullated bed purifier
The assembly dia is 2.4m, and height is about 6m, installation three phase separator at the top of device, recycling filter during for backwashing Material, while will be arranged outside counter-flushing liquid and backwash nitrogen;Filtrate is the quartz sand of 0.2mm~3mm, anthracite, shell, work in bed Property charcoal, alumina particle, carbon ball or Ceramic Balls equal sphere granule filter material, wherein filtering material particle shape also can be used column, four sides The irregular shapes such as body, better, bed height is 0.8~1.5m, and separate unit treating capacity is 50m3/ h, 6 are used in parallel, and 2 One group of platform, in turn switching backwash.
4. implementation process
Methanol-to-olefins washing water containing catalyst fines by centrifugal pumping to mini-hydrocyclone separation device initial gross separation, then into Enter ebullated bed separator group, remove fine particle in water;Ebullated bed separator group is 6 three groups of parallel operations, and 1 spare, even After reforwarding row is increased to 0.2MPa to pressure difference, backwash is switched in turn, is just washing operation, continues thereafter with operation.
5. experimental result
Specific separation situation is as shown in table 1 below:
Table 1:Separation parameter
By table 1 as it can be seen that after backwash boiling regeneration, seed activity is preferably lifted, design parameter such as table 2 below institute Show:
2 backwashing parameters of table
Pilot scale is filtered Pilot scale backwashes
Handle water 35~65m3/h 45~90m3/h
Solid content 50mg/l Less than 5%
Flow velocity 8~15m/h 10~20m/h
Catalyst residual rate -- More than 3.2%
Above-mentioned listed embodiment is only the preferred embodiment of the utility model, is not used for limiting the utility model Practical range.The equivalence changes and modification that i.e. all contents according to the application the scope of the claims are made, all should be the utility model Technology category.
It is incorporated herein by reference in all documents that the utility model refers to, just as each document quilt It is individually recited as reference.In addition, it should also be understood that, after the above-mentioned instruction content of the utility model has been read, this area skill Art personnel can make various changes or modifications the utility model, and such equivalent forms equally fall within the application appended claims Book limited range.

Claims (7)

1. a kind of MTO washes the hydraulic art continuous cycle of operation extended device, it is characterised in that the device includes:
Mini-hydrocyclone separation device (5), for MTO washing waters to be carried out micro- eddy flow processing, to remove the free oil in water removal;
The ebullated bed separator (7) being connected with mini-hydrocyclone separation device (5), for handling the washing water after micro- cyclone deoiling, with Remove oil emulsion, dispersed oil and catalyst fines.
2. device as claimed in claim 1, it is characterised in that the device further includes:
The settling tank (6) being connected with mini-hydrocyclone separation device (5), the washing water for being discharged to mini-hydrocyclone separation device (5) sink Drop, realizes water-oil separating;
The surge tank (8) being connected with ebullated bed separator (7), for storing through ebullated bed separator (7) purified washing water;
The stripping tower (10) being connected with surge tank (8), for the washing water handled through ebullated bed separator (7) to be carried out at stripping Reason.
3. device as claimed in claim 1 or 2, it is characterised in that the ebullated bed separator (7) for three phase separator and The combination of grain bed, medium used are more size Multiple Shape tandem compounds of granule filter material.
4. device as claimed in claim 3, it is characterised in that the particle selected in the grain bed medium, its particle size slope After change 50% or higher, increase with particle rotation intensity under flow, rotation turn up 1500rad/s or higher, particle layers Regeneration efficiency improves.
5. device as claimed in claim 1 or 2, it is characterised in that the operating temperature of the MTO washing waters is for 85 DEG C or more Height, the content of solid catalyst particle is 0.1~1.0g/L, and the average grain diameter of solid catalyst particle is 0.5~5 μm, washing Oil content in water is 200~700mg/L.
6. device as claimed in claim 5, it is characterised in that after being handled through ebullated bed separator, in washing water in oil phase Water content be down to less than 10%, oil content is down to below 30mg/L, and solid suspension content is down to below 20mg/L.
7. device as claimed in claim 1 or 2, it is characterised in that the use of medium is that particle diameter is 0.2mm~3mm in grain bed Polymorphic shape granule filter material, wherein ball-type rate is lower, particle diameter is smaller, and dirty rate of receiving is higher;Ball-type rate is higher, particle diameter is bigger, from It is higher to turn regeneration efficiency.
CN201721093388.XU 2017-08-29 2017-08-29 MTO washes the hydraulic art continuous cycle of operation extended device Active CN207313271U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201721093388.XU CN207313271U (en) 2017-08-29 2017-08-29 MTO washes the hydraulic art continuous cycle of operation extended device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201721093388.XU CN207313271U (en) 2017-08-29 2017-08-29 MTO washes the hydraulic art continuous cycle of operation extended device

Publications (1)

Publication Number Publication Date
CN207313271U true CN207313271U (en) 2018-05-04

Family

ID=62384538

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201721093388.XU Active CN207313271U (en) 2017-08-29 2017-08-29 MTO washes the hydraulic art continuous cycle of operation extended device

Country Status (1)

Country Link
CN (1) CN207313271U (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111115742A (en) * 2019-12-30 2020-05-08 华东理工大学 Method and device for removing halogenated hydrocarbon solvent from underground water

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111115742A (en) * 2019-12-30 2020-05-08 华东理工大学 Method and device for removing halogenated hydrocarbon solvent from underground water
CN111115742B (en) * 2019-12-30 2022-07-26 华东理工大学 Method and device for removing halogenated hydrocarbon solvent from underground water

Similar Documents

Publication Publication Date Title
CN108328761A (en) MTO washes the method and device of hydraulic art continuous operation cycle stretch-out
CN107382654B (en) Separation method and device for quenching water boiling bed for preparing olefin from methanol
CN107433055B (en) Boiling granules regeneration method and device in ebullated bed separator
CN107720872B (en) Purifying device and purifying method for washing water of methanol-to-olefin device
CN102093153A (en) Optimal combination method and device for purifying and separating MTO (Methanol To Olefins) reaction gas containing catalyst micropowder
CN107512787A (en) Medium sort method is separated in ebullated bed separator
CN207313271U (en) MTO washes the hydraulic art continuous cycle of operation extended device
CN102092886B (en) Combined sewage treatment method for oil field
WO2022056775A1 (en) Deep purification device and method for methanol-to-olefin washing water
JP4735262B2 (en) Cleaning method for solid particles
CN113045376A (en) Method and device for purifying methanol-to-olefin purified water by fluidized bed
CN211664891U (en) Deep purification device for methanol-to-olefin washing water
CN110550844A (en) Domestic sewage's processing system
CN207330792U (en) Methanol-to-olefins chilled water (chw) ebullated bed separator
Chen et al. Industrial application of swirl regenerating micro-channel separation (SRMS) for fine catalysts removal from methanol-to-olefin quench water
CN102232008B (en) Method and system for handling slurries of varying liquid rates and solids content
CN103706378B (en) Dead catalyst concentrate drying that in preparing isobutene through dehydrogenation of iso-butane, isobutene. is carried secretly and the processing method and processing device of removing toxic substances
Liu et al. Cooperative physical separation of oil and suspended solids from methanol-to-olefin wastewater: A pilot study
CN101795980B (en) Method for treatment of water comprising non-polar compounds
CN205590371U (en) MTOMTP chilled water (chw) of low energy consumption and membrane treatment equipment of washing water
CN115745075A (en) Method and device for purifying ethylene cracking furnace burning tail gas spray wastewater
CN104649446A (en) Liquid-solid separation method and device for MTO (methanol to olefins) quenching water and washing water
CN207619145U (en) A kind of sewage purification processing system
CN112272657B (en) Natural water and waste water treatment method
CN208054965U (en) A kind of methanol-to-olefins device washing water purifying means

Legal Events

Date Code Title Description
GR01 Patent grant
GR01 Patent grant