CN1233453C - Automatic filtering/back purging system liquid and solid separation for in three phase paste state bed reactor - Google Patents
Automatic filtering/back purging system liquid and solid separation for in three phase paste state bed reactor Download PDFInfo
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- CN1233453C CN1233453C CN 03150742 CN03150742A CN1233453C CN 1233453 C CN1233453 C CN 1233453C CN 03150742 CN03150742 CN 03150742 CN 03150742 A CN03150742 A CN 03150742A CN 1233453 C CN1233453 C CN 1233453C
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Abstract
The present invention relates to an automatic filtering/back flushing system for the liquid-solid separation of a three-phase slurry state bed reactor, which is divided into a filtering unit, a liquid processing unit and a back flushing unit, wherein the filtering unit is composed of 1 to 5 layers of first grade liquid-solid separation devices arranged in the reactor; the liquid processing unit comprises a liquid collecting tank; back flushing mediums in the back flushing unit can be liquid or gas, wherein a liquid back flushing unit comprises a back flushing liquid collecting tank, and a gas back flushing unit comprises a back flushing gas jar. Compared with the prior art, the present invention has the characteristics of reasonable structure and clogging prevention, and can guarantee the continuous and normal operation of the reactor.
Description
Technical field
The present invention relates to a kind of device that in the three phase slurry bed bioreactor of continued operation, solid fine grained and liquid phase is carried out automatic fitration/recoil, be applicable to the process of using the three phase slurry bed bioreactor to react, as Fischer-Tropsch building-up process from the synthesis gas preparation hydrocarbon fuels.
Background technology
Three-phase bed reactor has obtained extensive use in current chemical process, for the very big catalytic reaction process of reaction heat, use three-phase bed reactor can effectively remove reaction heat, and the isothermal operation of realization response device guarantees the normal operation of reactor.Three-phase bed reactor commonly used is a paste state bed reactor, comprises mechanical agitation suspension reactor and bubbling suspension reactor.
For the process (as the Fischer-Tropsch building-up process) that generates product liquid, the slurries that contain finely grained catalyst in the phase reactor must carry out liquid-solid separation to obtain product liquid, desirable liquid-solid separation process should be carried out in reactor, be about to liquid and shift out reactor, but catalyst granules is stayed in the reactor; And for liquid be the process (as generate the process of oxygenatedchemicals with synthesis gas) of inert media liquid also must regularly shift out and add so that the impurity in the liquid maintains certain level.
The liquid-solid separation of the catalyst slurry of the three phase slurry bed bioreactor reactor of being everlasting carries out outward, and the conveying of suspension must use specific pump to carry out, and the catalyst that filters still need turn back in the reactor with the slurries form.This process is easy to cause the breakage of catalyst granules, thereby the long-time continuous operation of reactor is brought problem.
Liquid-solid separation device for the inside setting, in one piece of report of USDOE once to Fischer-Tropsch synthetic pulp state bed reactor in the problem of dope filtration analyze, think that the liquid-solid separation device that is arranged on inside reactor will the very fast obstruction along with the growth of filtration time, cause outage.
At this report, Den Norske Stats Oljeselskap a.s. (Statoil Group) has proposed a kind of solid-liquid suspended substance treatment facility and heterogeneous catalytic reaction equipment at one piece of Chinese patent (application number 9410116.X), this equipment is the liquid-solid separation device that is arranged on inside reactor, its main characteristics be this equipment by will leach the district with reaction zone between be communicated with, can prevent that solid matter from generating on filter element.But the equipment that this patent provides still has very big deficiency, the one, and complex structure will cause maintenance difficult like this; The 2nd, owing to clearly do not propose the automatic backwash measure of sequencing, still can't avoid the very fast obstruction of growth along with filtration time, cause the problem of outage.
Summary of the invention
Purpose of the present invention be exactly provide in order to overcome the defective that above-mentioned prior art exists a kind of rational in infrastructure, avoid stopping up, can guaranteeing the reactor automatic fitration/recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor of normal operation continuously.
Purpose of the present invention can be achieved through the following technical solutions: a kind of automatic fitration/recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor is characterized in that this device comprises three parts: filter element, liquid-treatment unit and back flush unit; Described filter element is made up of 1～5 layer of one-level liquid-solid separation device that is arranged in the reactor, and every layer of liquid-solid separation device comprises 1～50 bank of filter elements; Described liquid-treatment unit comprises at least one liquid collection trough and at least one cover secondary liquid-solid separation device and supporting liquid delivery pump thereof; Described back flush unit is used for the washing and filtering element, used recoil medium adopts liquid, or employing gas, described employing liquid comprises at least one backflush liquid feeder and at least one backflush liquid groove that is used to provide backflush liquid as the liquid back flush unit of recoil medium, perhaps comprise at least one backflush liquid feeder and at least one backflush liquid pump, described employing gas comprises at least one recoil gas tank as the gas backwash unit of recoil medium; Described every group of filter element disposes one group of filtration/recoil valve, comprise a Filter valve and a recoil valve, this Filter valve is separately positioned on the outer house steward up and down who links to each other with filter cell of reactor with the recoil valve, and the motive force of described filtration comes from the pressure reduction between reactor and the liquid collection trough.
In the described filter element, every bank of filter elements is made up of 1～40 tube filtering element arranged side by side again, and tube filtering element arranged side by side is combined by up and down two connecting pipes and 2～80 groups of conduit couplings, is connected on the outer house steward of reactor.
Described liquid-treatment unit also comprises at least one filter liquide cooler and/or at least one fluid cushion groove.
The described backflush liquid feeder and being used to of comprising provides the liquid back flush unit of the backflush liquid groove of backflush liquid to comprise that also at least one is used for backflush liquid is heated to backflush liquid heater near temperature of reactor, backflush liquid washes the filter element in the reactor by the pressure reduction between backflush liquid groove and the reactor, at least one backflush liquid pump is set, to replenish the liquid that is used to recoil in the backflush liquid feeder before the backflush liquid groove.
The described liquid back flush unit that comprises backflush liquid feeder and backflush liquid pump comprises that also at least one is used for liquid is heated to backflush liquid heater near temperature of reactor, and backflush liquid washes the filter element in the reactor by the pressure that the backflush liquid pump provides.
Described gas backwash unit comprises that also at least one is heated to back flushing air body heater near temperature of reactor with gas, recoil gas is the gas identical with reacting gas, or different with it inert gases, recoil gas washes the filter element in the reactor by the pressure reduction between recoil gas tank and the reactor.
Described liquid collection trough is in reactor downstream, operating temperature and pressure ratio reactor are lower slightly, be used for the liquid behind the receiving filtration, often need establish liquid heat tracing facility, the control valve that liquid collection trough pressure is put on the pipeline by speeding is regulated, or increase other gas line, realize the branch process control of pressure by the adjusting of this gas addition and the discharge quantity of speeding.
Described fluid cushion groove the liquid that is used to collect from liquid collection trough, operating temperature and pressure are according to fed distance, post processing requires decision, and operating temperature should be higher 20～50 ℃ than the freezing point of liquid at least, as required if do not establish liquid heat tracing facility, when the pressure of liquid collection trough is higher, this dashpot also is used to cool off the vacuum flashing of back liquid, the control valve that dashpot pressure is put on the pipeline by speeding is regulated, or increase other gas line, realize the branch process control of pressure by the adjusting of this gas addition and the discharge quantity of speeding, when the three-phase bed reactor operating temperature is higher, the filter liquide cooler need be set before the fluid cushion jar.
Described secondary liquid-solid separation device and the supporting with it liquid delivery pump of liquid being done further filtration, consider to be when standby many covers, liquid delivery pump be arranged on before the secondary liquid-solid separation device and the fluid cushion groove after, only need to consider the compensation filtration pressure difference and provide enough lifts with the backflush liquid feeder the battery limit (BL) outside for liquid is transported to; The setting of described secondary liquid-solid separation device is to remove for the subparticle that may carry secretly in the one-level liquid-solid separation device liquid in the future autoreactor, for the back flush unit that with liquid is the recoil medium, the concentration of contained solid particle in the liquid behind the cascade filtration, be 1～100ppm, cause the obstruction of liquid-solid separation device inner filter element when preventing to recoil.
After described backflush liquid feeder is arranged on the secondary liquid-solid separation device, be used to collect the liquid that is used to recoil, its operating temperature is identical with secondary liquid-solid separation device outlet temperature, operating pressure then depends on follow-up equipment, the control valve that the pressure of backflush liquid feeder is put on the pipeline by speeding is regulated, also increase other gas line, realize the branch process control of pressure by the adjusting of this gas addition and the discharge quantity of speeding; Described secondary liquid-solid separation device outlet is divided into two-way, and a part of carrying device goes to the subsequent treatment unit, and another part is sent to the backflush liquid feeder as recoil liquid; Before described backflush liquid groove is positioned at reactor, realize the branch process control of pressure by gases at high pressure addition and the adjusting of discharge quantity of speeding, the pressure of backflush liquid groove should be higher than reactor pressure 0.1～1.0Mpa; The backflush liquid pump places after the backflush liquid feeder, is used to carry the filter cell in the backflush liquid flushing reactor, and when the non-recoil liquid tank, the backflush liquid pump must satisfy the requirement of rapid start and stop and frequent starting; When backflush liquid need heat, the backflush liquid heater was heated to highly pressurised liquid near temperature of reactor with heat medium before placing the backflush liquid groove.
Described secondary liquid-solid separation device exports whole carrying devices and goes to the subsequent treatment unit; Before described recoil gas tank was positioned at reactor, pressure was realized the branch process control by the adjusting of the gases at high pressure addition and the discharge quantity of speeding, and the pressure of recoil gas tank should be higher than reactor pressure 0.1～1.0Mpa; Need heat the time, the back flushing air body heater places on the pressurized gas inlet pipeline of recoil gas tank at recoil gas, with heat medium gases at high pressure is heated to temperature near reactor.
The present invention is applicable to the particle of handling 1-250 μ m, and the concentration of solid particle in slurries is the system of 5～50wt%, but the particle that exceeds this particle size range is also had treatment effect preferably.In fact, because bigger greater than the particle inside diffusional resistance of 250 μ m less than the particle of 1 μ m is easy to be taken out of by gas phase in the reactor, 1-250 μ m also is the general three phase slurry bed bioreactor granularity requirements to catalyst.
The characteristics of automatic fitration/recoiling device that the present invention adopts are, periodically filter element are recoiled, and by to the control of pressure reduction with to the adjustment of filtration, recoil and time of repose, effectively suppress the gathering of solid particle on the filter filter opening.Owing to have rationally and the filtration of sequencing/recoil setting, can move for a long time and blockage problem can not occur.And what adopt is detachable internal ramp element, is convenient to maintenance.This invention has well solved the problem that prior art exists.
Device of the present invention is divided into three parts: filter element, liquid-treatment unit and back flush unit.
Filter element is made up of 1～5 layer of one-level liquid-solid separation device that is arranged in the reactor.Every layer of liquid-solid separation device comprises 1～50 bank of filter elements, and every bank of filter elements is made up of 1～40 filter cell again.Liquid-treatment unit comprises and is used to collect the liquid collection trough that filters gained liquid, optionally is used for the filter liquide cooler of cooling liquid, secondary liquid-solid separation device and the supporting with it liquid delivery pump that is used to collect the fluid cushion groove of cooling back liquid and liquid is done further purify.Back flush unit adopts the difference of liquid or gas can be divided into liquid back flush unit and gas back flush unit according to the recoil medium.For the liquid back flush unit, generally comprise backflush liquid feeder, optional backflush liquid heater, backflush liquid pump and optional backflush liquid groove; For the gas backwash unit, generally comprise recoil gas tank and optional gas heater.Three unit to device of the present invention describe respectively below.
(1) filter element
Every bank of filter elements structure provided by the invention is many tube filtering elements arranged side by side, combines by connecting pipe and connector, and the factors such as need taking all factors into consideration built-in filter quantity and cross section layout that is provided with of filter element quantity arranged side by side determines.Every group of filter element disposes one group of filtration/recoil valve, and valve is arranged on the house steward that reactor is outer with filter cell links to each other.The recoil valve is on last house steward, and Filter valve is on following house steward.Or in contrast, the recoil valve is on following house steward, and Filter valve is on last house steward.
The objective of the invention is to, the liquid that reaction is generated or join in the reactor from the outside shifts out reactor, and the realization solid separates with liquid, realizes the control to the reactor liquid level simultaneously.Therefore, quantity and the pressure reduction between liquid collection trough and the reactor that is used to the filter element that filters is determined by the height of liquid level.When liquid level is too high, filter element quantity that the need increase is used to filter or the pressure reduction between increasing reactor and the liquid collection trough.Cross when low when liquid level, need to reduce the quantity of the filter cell that is used to filter or the pressure reduction between reactor and the liquid collection trough.
The motive force of filtering comes from the pressure reduction between reactor and the liquid collection trough.When the pressure reduction between reactor and the liquid collection trough was higher, filtered driving force was big, and the rate of filtration is fast, and promptly filtering traffic is big; On the contrary, when pressure reduction was low, filtered driving force was little, and the rate of filtration is slow, and promptly filtering traffic is little.
Automatic fitration of the present invention/recoil control program can manually pin any filter element group in advance, and removes one or more filter element groups from program, and remaining filter element group will continue normal operation.Be in operating filter element group and will be carried out required recoil and filter set by step by orderization ground.Thereby be implemented in the normal running, some filter element is in the filtration state, and some filter element is in the recoil state, and some filter element is in two static conditions between the cycle.Wherein, filtration step comprises the recoil valve of closing backflush liquid, opens the Filter valve of same filter element group simultaneously; The recoil step comprises the Filter valve of closing the filter liquide outlet, opens the recoil valve of same filter element group simultaneously, thereby with a higher fluid recoil impulse filter element is carried out backwash; Comprise the recoil and the Filter valve of closing same filter element group simultaneously and leave standstill step.
Because online number of filters is variable, so the total flow of filter liquide is a kind of from the continually varying flow summation of carrying out the filter cell that filters.And owing to depend on the differential pressure between the liquid collection trough in the reactor and liquid-treatment unit under the filtration state from the size of fluid flow of each group filter element, so the big young pathbreaker of total logistics is determined by the quantity of the filter cell that is in the filtration state and the pressure reduction between the liquid collection trough in reactor and the liquid-treatment unit.
(2) liquid-treatment unit
Liquid-treatment unit comprises following equipment:
Liquid collection trough.Be in reactor downstream, operating temperature and pressure ratio reactor are lower slightly, are used for liquid behind the receiving filtration, often need establish liquid heat tracing facility, and quantity is at least one.The control valve that feeder pressure is put on the pipeline by speeding is regulated, and also can increase the pipeline of other gases, realizes the branch process control of pressure by the adjusting of this gas addition and the discharge quantity of speeding.
Optional filter liquide cooler.Select for use when the paste state bed reactor temperature is higher, quantity is at least one, and is lower as the three-phase bed reactor operating temperature, and this filter liquide cooler can be ignored.Be arranged between liquid collection trough and the fluid cushion groove, liquid cools arrived the operating temperature of fluid cushion groove with cooling medium.
The fluid cushion groove.Be used to collect liquid from liquid collection trough, operating temperature and pressure require decision according to fed distance, post processing, and operating temperature should be higher 20～50 ℃ than freezing point at least, and quantity is at least one.Pressure as liquid collection trough is higher, this dashpot also can be used for cooling off the vacuum flashing of back liquid, the control valve that dashpot pressure is put on the pipeline by speeding is regulated, also can increase the pipeline of other gases, realize the branch process control of pressure by the adjusting of this gas addition and the discharge quantity of speeding.
Liquid is made further secondary liquid-solid separation device and the supporting with it liquid delivery pump that filters, and quantity is at least one cover.Liquid delivery pump be arranged on before the secondary liquid-solid separation device and the fluid cushion groove after, general only need to consider the compensation filtration pressure difference and be transported to the lift that provides enough outside the battery limit (BL) for liquid, if back flush unit is the recoil medium with liquid, the backflush liquid feeder that also need be thought of as back flush unit provides transmitting power.The secondary liquid-solid separation device is removed the subparticle in the liquid, for the liquid back flush unit that with liquid is the recoil medium, the outlet of secondary liquid-solid separation device is divided into two-way, the part carrying device goes to the subsequent treatment unit, part is sent to the backflush liquid feeder and is used as backflush liquid, behind the cascade filtration in the liquid concentration of contained solid particle must meet certain requirements, be generally 1-100ppm, cause the obstruction of filter element to prevent backflush liquid from bringing solid particle into.For the gas backwash unit, the battery limit (BL) is directly sent in the outlet of secondary liquid-solid separation device, and the concentration of contained solid particle in the liquid generally is not strict with.
(3) back flush unit
For the liquid back flush unit, this unit is associated with liquid-treatment unit, can adopt a kind of of following two kinds of forms:
Back flush unit is made up of at least one backflush liquid feeder, at least one backflush liquid pump and at least one optional backflush liquid heater.Backflush liquid washes the filter element in the reactor by the pressure that the backflush liquid pump provides.
Back flush unit is made up of at least one backflush liquid feeder, at least one backflush liquid groove, at least one backflush liquid pump and at least one optional backflush liquid heater.Backflush liquid washes the filter element in the reactor by the pressure reduction between backflush liquid groove and the reactor.
For the gas backwash unit, this unit and liquid-treatment unit are independent, are made up of at least one recoil gas tank and optional back flushing air body heater.The gas of recoil usefulness can adopt the process gas of synthetic usefulness, also can adopt inert gas.Recoil gas washes the filter element in the reactor by the pressure reduction between recoil gas tank and the reactor.
Back flush unit comprises following equipment:
The backflush liquid feeder.After placing the secondary liquid-solid separation device of liquid-treatment unit, collect the liquid that is used to recoil.Its operating temperature is general identical with secondary liquid-solid separation device outlet temperature.Operating pressure then depends on follow-up equipment (before advancing reactor).The control valve that backflush liquid feeder pressure is put on the pipeline by speeding is regulated, and also can increase the pipeline of other gases, realizes the branch process control of pressure by the adjusting of this gas addition and the discharge quantity of speeding.
Backflush liquid heater or back flushing air body heater.Lower as the three-phase bed reactor operating temperature, can not establish these heating heat exchangers.The effect of these heat exchangers is that the recoil medium is heated near temperature of reactor.For the liquid back flush unit, before use backflush liquid heater places reactor; For the gas backwash unit, use the back flushing air body heater to place on the recoil gas suction line of recoil gas tank.
The backflush liquid pump.Place after the backflush liquid feeder, if back non-recoil liquid tank, the backflush liquid pump should be able to satisfy the requirement of rapid start and stop and frequent starting.
The backflush liquid groove.Before being positioned at reactor, pressure is realized the branch process control by the adjusting of the gases at high pressure addition and the discharge quantity of speeding, and generally is higher than reactor 0.1～1.0MPa.
The recoil gas tank.Before being positioned at reactor, pressure is realized the branch process control by the adjusting of the high pressure recoil gas addition and the discharge quantity of speeding, and generally is higher than reactor 0.1～1.0MPa.
For guaranteeing the reliable and stable and long operation of automatic fitration/recoiling device.In the control program of automatic fitration/recoiling device, also need to do following setting
Reactor liquid level and filtration/recoil is provided with
When the reactor liquid level is higher than high liquid level, need to increase the quantity of opening Filter valve, the quantity of the filter element that is used to filter with increase; When liquid level is lower than liquid level, need close some Filter valves, the filter element quantity that is used to filter with minimizing.When liquid level is lower than liquid level, will stop filtration/recoil program automatically, closeall filtration and recoil valve, promptly all filter cells all are in static condition, return to low liquid level until liquid level, just restart filtration/recoil program, open automatically and filter and the recoil valve.When liquid level is higher than high liquid level, stop the recoil program, closeall recoil valve, between 10～30min time delay, filter element is in the filtration state always, if when liquid level drops to high liquid level, recovers the recoil program, opens the recoil valve.
Differential pressure and filtration between reactor and the liquid collection trough/recoil is provided with
When the pressure reduction between reactor and the liquid collection trough sets value less than a certain low level, need close the filter element quantity that some Filter valves are used to filter with minimizing.When pressure reduction sets value greater than an a certain high position, the filter element quantity that the quantity that needs increase to open Filter valve is used to filter with increase.If occur high head pressure between reactor and the liquid collection trough, will stop the recoil program, closeall recoil valve, during 10～30min time-delay is filtered, in case the pressure reduction between reactor and the liquid collection trough less than head pressure after, the recoil valve is opened automatically, recovers the recoil program.
Differential pressure and filtration/recoil are provided with between reactor and the backflush liquid groove (if being that the used recoil medium of back flush unit is a liquid)
Pressure reduction between reactor and the backflush liquid groove is if low low differential pressure, and with closeall recoil valve, promptly all filter cells are no longer accepted backwash.Between 10～30min time delay, to accept without any filter element under the situation of backwash, filter element will be in the filtration state always.When in a single day differential pressure was increased to greater than low differential pressure, device recovered to open the recoil program automatically.
The interlocking of backflush liquid pump (if back flush unit does not comprise the backflush liquid groove)
In these cases, if the condition of recoil valve closing occurs, the backflush liquid pump needs out of service.When waiting to occur to recoil the condition of valve opening, the backflush liquid pump restarts.The backflush liquid pump should satisfy the requirement that repeats repeatedly start and stop, and the backflush liquid pump lift is by the pressure decision of reactor.
The control (if the used recoil medium of back flush unit is a gas) of differential pressure between reactor and the recoil gas tank
Pressure reduction between reactor and the recoil gas tank is if low low differential pressure, and with closeall recoil valve, promptly all filter cells are no longer accepted backwash.Between 10～30min time delay, to accept without any filter element under the situation of backwash, filter element will be in the filtration state always.When in a single day differential pressure was increased to greater than low differential pressure, device recovered to open the recoil program automatically.
Description of drawings
Fig. 1 is the layout schematic diagram of filter cell on reactor cross-section;
Fig. 2 is that a bank of filter elements and filtration/recoil valve thereof are provided with schematic side view;
Fig. 3 is for adopting the Fischer-Tropsch compound probability experimental rig paraffin filtration/recoiling device schematic diagram of liquid as the recoil medium;
Fig. 4 is for adopting the Fischer-Tropsch compound experiment chamber device paraffin filtration/recoiling device schematic diagram of liquid as the recoil medium;
Fig. 5 is for adopting the Fischer-Tropsch compound probability experimental rig paraffin filtration/recoiling device schematic diagram of gas as the recoil medium.
The specific embodiment
The present invention can be achieved by the whole bag of tricks, at first in conjunction with a paraffin filtration/recoiling device example in Fischer-Tropsch compound probability experimental rig, consults Fig. 1～Fig. 3 and describes below.
The Fischer-Tropsch synthesizer is to utilize synthesis gas, and Fischer-Tropsch is synthetic carrying out in slurry attitude bed under the effect of catalyst and under 200～250 ℃, the operating condition of 2.0～5.0MPa, generates a series of hydrocarbon compound.Hydrocarbon compound obtains thick product after Quench, flash distillation, separation, filtration: heat is coagulated oil, cold oil and wax.Wherein paraffin is as the liquid medium in the reactor, is again the important products of synthesizing.
The six bank of filter elements groups 13 that shown in Figure 1 is on reactor 12 cross sections evenly distribute on the cross section, and wherein, every bank of filter elements 13 is three tubular filters 14 arranged side by side.The distance of filter cell group 13 distance centers needs according to reactor 12 and the decision of filter cell group 13 sizes.
Fig. 2 is for by shown in the side direction view being a bank of filter elements 13 and filtrations/recoil valve 19 thereof and 20 settings.Three tubular filters 14 arranged side by side are by two communicating pipe 17 and six groups of flanges 16 are combined up and down, be connected to up and down two by flange 17 again and be communicated on the outer house steward 18 of reactor, such be arranged so that when guaranteeing built-in filter quantity that perforate is less on the reactor.Every group of filter element disposes one group of filtration/ recoil valve 19 and 20, is arranged on the house steward 18 that reactor is outer with filter cell group 13 links to each other, and recoil valve 19 is on last house steward, and Filter valve 20 is on following house steward.
As shown in Figure 3, in reactor 1, the paraffin that reaction produces is disposed to paraffin feeder 3 after inside reactor filter 2 (being the one-level liquid-solid separation device) filters, enter then and enter 5 flash distillations of paraffin dashpot after scale wax cooler 4 is cooled to 110～150 ℃.Paraffin after the flash distillation filters a back part by scale wax pump 6 through paraffin press 7 (being the secondary liquid-solid separation device) and enters recoil paraffin feeder 8, again through 9 pressurizations of recoil paraffin pump, paraffin wax product heater 10 is heated to 200～240 ℃ and sends into recoil paraffin tank 11, as the recoil paraffin of reactor.Wherein, several groove jars are all realized the branch process control of pressure by the adjusting of the nitrogen addition and the discharge quantity of speeding.
12 bank of filter elements are divided into two-layer (comprising 12 pairs of filtration/recoil valves, totally 24 valves), are placed on Fischer-Tropsch synthesis device inside, are used for isolating or block catalyst entering in the paraffin that flows in the paraffin feeder 3.Every group of valve comprises a former wax Filter valve and a recoil wax valve.These valves will be carried out required recoil and filter set by step by orderization ground.In the present embodiment, remove to control filtration/recoil valve of every layer respectively with two filtration/recoil programs, whole recoil program circulation primary had for 6 steps, for every pair of valve (imported valve and an outlet valve are formed), in each step, can divide three substeps again, promptly filter, recoil, leave standstill the stage.
One is in valve sets under the filter operation state through an adjustable filtration time (10～40 minutes) afterwards, will enters the recoil state in order.The recoil step comprises the Filter valve of closing a former wax outlet; Open simultaneously the recoil wax valve of a former wax inlet at short notice, advanced this valve with the flow velocity of a higher paraffin recoil impulse formula.Recoil paraffin tank 11 is carried out pressure control, keep the differential pressure certain, to satisfy certain static pressure pulse requirement with reactor 1.This recoil valve also is (2～20 seconds) that can regulate from being opened to each burst length of closing.Allow 3 pulse processes in the recoil program, wherein 2 times is the usefulness that is about to from the valve sets that is filled into static condition; Supply with the usefulness that is about to from the valve sets that leaves standstill to the state of filtration 1 time.The big young pathbreaker of blanking time between these valves is depended on what of quantity of the Filter valve under the presence.
Occur at certain filter under the situation of catalyst breakage, valve can keep in repair, and gets rid of outside program, continues then last Filter valve is turned round.Therefore total flow is a kind of total compound of the continuous variable flow from different Filter valves.And the speed of flow depends on the quantity of the filter cell that is in the filtration state and the pressure reduction of reactor and paraffin feeder.
In case of emergency, can automatically reset and hand-reset, program will turn back to the filtration initial state again.
The time of filtering/recoil/leaving standstill is traditionally arranged to be: filtered 10～40 minutes, once recoil was 2 seconds.Leave standstill is 10 minutes.
(1) control of reactor 1 liquid level:
When liquid level is higher than high liquid level, need to increase the quantity of opening Filter valve; When liquid level is lower than liquid level, need close some Filter valves.Closing or opening of these valves can manually or automatically perform.When liquid level is lower than liquid level, will stop filtration/recoil program automatically, closeall filtration and recoil valve return to low liquid level until liquid level, just restart filtration/recoil program, open automatically and filter and the recoil valve.When liquid level is higher than high liquid level, stop the recoil program, closeall recoil valve, between the 10min time delay, Filter valve filters always, if when liquid level drops to high liquid level, recovers the recoil program, opens the recoil valve.
(2) control of the differential pressure between reactor 1 and the paraffin feeder 3
Carrying out pressure reduction in 0.01～0.8MPa scope regulates; Pressure reduction need be closed some Filter valves during less than 0.01Mpa.Pressure reduction needs to increase the quantity of opening Filter valve during greater than 0.8Mpa.Closing or opening of these valves can manually or automatically perform.If high head pressure 1.2Mpa occurs, will stop the recoil program, closeall recoil valve, during the 10min time-delay is filtered, in case pressure less than head pressure 0.8Mpa after, all recoil valve goalkeepers open automatically, recover the recoil program.
(3) control of differential pressure between reactor 1 and the recoil paraffin tank 11
Pressure reduction is if low low differential pressure 0.2MPa, with closeall recoil valve.Between the 10min time delay, under the situation without any the recoil valve open, Filter valve will be in always and carry out the filtration state.When in a single day differential pressure was increased to greater than low differential pressure 0.3MPa, device recovered to open the recoil program automatically.
This commerical test device is used to handle the particle of 1-50 μ m, and the concentration of solid particle in slurries is 45wt%.This covering device operation half a year, to filter, the recoil stable operation, the situation of parking never appears causing because of obstruction, during Programmed Stop, take out filter cell, there is not particle aggregation on the filter opening substantially.
Present embodiment is a Fischer-Tropsch compound experiment chamber device paraffin filtration/recoiling device, and schematic flow sheet is seen the Fig. 4 in the accompanying drawing.
Present embodiment and embodiment 1 device difference are: back flush unit is formed the non-recoil paraffin tank by recoil paraffin feeder, recoil paraffin pump and heat exchanger.Owing to be laboratory installation, filter has only been established one deck, establishes four groups of valves altogether, and adopts the mechanical agitation suspension reactor, and what mode of heating adopted is electrical heating.
As shown in Figure 4, in reactor 1, the paraffin that reaction produces is disposed to paraffin feeder 3 after inside reactor filter 2 filters, enter then and enter 5 flash distillations of paraffin dashpot after scale wax cooler 4 is cooled to 110～150 ℃.Paraffin after the flash distillation filters a back part by scale wax pump 6 through paraffin press 7 and enters recoil paraffin feeder 8, is heated to 200～240 ℃ through recoil paraffin pump 9 by paraffin wax product heater 10 again and directly squeezes into reactor as recoil paraffin.
The setting of the filtration among this embodiment/recoil program is also substantially the same manner as Example 1, and difference mainly is not have the Self-control interlock between reactor and the recoil paraffin tank, has increased the interlocking of a recoil paraffin pump, and requiring of this interlocking is as follows:
In other interlocking condition, when the condition of recoil valve closing occurring, recoil paraffin pump needs out of service.When waiting to occur to recoil the condition of valve opening, recoil paraffin pump starts immediately, resumes operation.
The grain graininess that this experimental provision is handled is identical with embodiment 1, through repeatedly operation, each cycle is about 30 days, and operating process is stable, the sharply situation of rising does not appear in pressure reduction between reactor and the liquid collection trough, and the filter cell that disassembles after the parking does not have solid and assembles.
Present embodiment is for adopting the Fischer-Tropsch compound probability experimental rig gas backwash device of gas for the recoil medium, and schematic flow sheet is seen the Fig. 5 in the accompanying drawing.
Present embodiment is except that back flush unit, and is identical with embodiment 1.In the present embodiment, back flush unit is by recoil gas (nitrogen) heater 10 ' and recoil nitrogen pot 11 ' formation.
As shown in Figure 5, in reactor 1, the paraffin that reaction produces is disposed to paraffin feeder 3 after inside reactor filter 2 filters, enter then and enter 5 flash distillations of paraffin dashpot after scale wax cooler 4 is cooled to 110～150 ℃.Paraffin after the flash distillation is sent to subsequent treatment after being filtered through paraffin press 7 by scale wax pump 6, high pressure nitrogen through 200～240 ℃ of recoil nitrogen heaters 10 ' be heated to send into recoil nitrogen pot 11 ', as the recoil gas of reactor.Wherein, except that the recoil nitrogen pot, other several groove jars all adopt the high pressure nitrogen addition and the discharge quantity of speeding is regulated the branch process control that realizes pressure.And recoil nitrogen pot pressure only depends on the discharge quantity of speeding to be regulated.
The grain graininess that this commerical test device is handled is identical with embodiment 1, and the effect of moving is also fine, and stopping state does not appear in filter element in 60 days running.
Claims (11)
1. an automatic fitration/recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor is characterized in that, this device comprises three parts: filter element, liquid-treatment unit and back flush unit; Described filter element is made up of 1～5 layer of one-level liquid-solid separation device that is arranged in the reactor, and every layer of liquid-solid separation device comprises 1～50 bank of filter elements; Described liquid-treatment unit comprises at least one liquid collection trough and at least one cover secondary liquid-solid separation device and supporting liquid delivery pump thereof; Described back flush unit is used for the washing and filtering element, used recoil medium adopts liquid, or employing gas, described employing liquid comprises at least one backflush liquid feeder and at least one backflush liquid groove that is used to provide backflush liquid as the liquid back flush unit of recoil medium, perhaps comprise at least one backflush liquid feeder and at least one backflush liquid pump, described employing gas comprises at least one recoil gas tank as the gas backwash unit of recoil medium; Described every group of filter element disposes one group of filtration/recoil valve, comprise a Filter valve and a recoil valve, this Filter valve is separately positioned on the outer house steward up and down who links to each other with filter cell of reactor with the recoil valve, and the motive force of described filtration comes from the pressure reduction between reactor and the liquid collection trough.
2. automatic fitration/the recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 1, it is characterized in that, in the described filter element, every bank of filter elements is made up of 1～40 tube filtering element arranged side by side again, tube filtering element arranged side by side is combined by up and down two connecting pipes and 2～80 groups of conduit couplings, is connected on the outer house steward of reactor.
3. automatic fitration/the recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 1 is characterized in that, described liquid-treatment unit also comprises at least one filter liquide cooler and/or at least one fluid cushion groove.
4. automatic fitration/the recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 1, it is characterized in that, the described backflush liquid feeder and being used to of comprising provides the liquid back flush unit of the backflush liquid groove of backflush liquid to comprise that also at least one is used for backflush liquid is heated to backflush liquid heater near temperature of reactor, backflush liquid washes the filter element in the reactor by the pressure reduction between backflush liquid groove and the reactor, at least one backflush liquid pump is set, to replenish the liquid that is used to recoil in the backflush liquid feeder before the backflush liquid groove.
5. automatic fitration/the recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 1, it is characterized in that, the described liquid back flush unit that comprises backflush liquid feeder and backflush liquid pump comprises that also at least one is used for liquid is heated to backflush liquid heater near temperature of reactor, and backflush liquid washes the filter element in the reactor by the pressure that the backflush liquid pump provides.
6. automatic fitration/the recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 1, it is characterized in that, described gas backwash unit comprises that also at least one is heated to back flushing air body heater near temperature of reactor with gas, recoil gas is the gas identical with reacting gas, or different with it inert gases, recoil gas washes the filter element in the reactor by the pressure reduction between recoil gas tank and the reactor.
7. automatic fitration/the recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 1, it is characterized in that, described liquid collection trough is in reactor downstream, operating temperature and pressure ratio reactor are lower slightly, be used for the liquid behind the receiving filtration, often need establish liquid heat tracing facility, the control valve that liquid collection trough pressure is put on the pipeline by speeding is regulated, or increase other gas line, realize the branch process control of pressure by the adjusting of this gas addition and the discharge quantity of speeding.
8. automatic fitration/the recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 3, it is characterized in that, described fluid cushion groove the liquid that is used to collect from liquid collection trough, operating temperature and pressure are according to fed distance, post processing requires decision, and operating temperature should be higher 20～50 ℃ than the freezing point of liquid at least, as required if do not establish liquid heat tracing facility, when the pressure of liquid collection trough is higher, this dashpot also is used to cool off the vacuum flashing of back liquid, the control valve that dashpot pressure is put on the pipeline by speeding is regulated, or increase other gas line, realize the branch process control of pressure by the adjusting of this gas addition and the discharge quantity of speeding, when the three-phase bed reactor operating temperature is higher, the filter liquide cooler need be set before the fluid cushion jar.
9. automatic fitration/the recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 1, it is characterized in that, described secondary liquid-solid separation device and the supporting with it liquid delivery pump of liquid being done further filtration, consider to be when standby many covers, liquid delivery pump be arranged on before the secondary liquid-solid separation device and the fluid cushion groove after, only need to consider the compensation filtration pressure difference and provide enough lifts with the backflush liquid feeder the battery limit (BL) outside for liquid is transported to; The setting of described secondary liquid-solid separation device is to remove for the subparticle that may carry secretly in the one-level liquid-solid separation device liquid in the future autoreactor, for the back flush unit that with liquid is the recoil medium, the concentration of contained solid particle in the liquid behind the cascade filtration, be 1～100ppm, cause the obstruction of liquid-solid separation device inner filter element when preventing to recoil.
10. automatic fitration/the recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 1, it is characterized in that, after described backflush liquid feeder is arranged on the secondary liquid-solid separation device, be used to collect the liquid that is used to recoil, its operating temperature is identical with secondary liquid-solid separation device outlet temperature, operating pressure then depends on follow-up equipment, the control valve that the pressure of backflush liquid feeder is put on the pipeline by speeding is regulated, or increase other gas line, realize the branch process control of pressure by the adjusting of this gas addition and the discharge quantity of speeding; Described secondary liquid-solid separation device outlet is divided into two-way, and a part of carrying device goes to the subsequent treatment unit, and another part is sent to the backflush liquid feeder as recoil liquid; Before described backflush liquid groove is positioned at reactor, realize the branch process control of pressure by gases at high pressure addition and the adjusting of discharge quantity of speeding, the pressure of backflush liquid groove should be higher than reactor pressure 0.1～1.0Mpa; The backflush liquid pump places after the backflush liquid feeder, is used to carry the filter cell in the backflush liquid flushing reactor, and when the non-recoil liquid tank, the backflush liquid pump must satisfy the requirement of rapid start and stop and frequent starting; When backflush liquid need heat, the backflush liquid heater was heated to highly pressurised liquid near temperature of reactor with heat medium before placing the backflush liquid groove.
11. the automatic fitration/recoiling device that is used for the liquid-solid separation of three phase slurry bed bioreactor according to claim 1 is characterized in that, described secondary liquid-solid separation device exports whole carrying devices and goes to the subsequent treatment unit; Before described recoil gas tank was positioned at reactor, pressure was realized the branch process control by the adjusting of the gases at high pressure addition and the discharge quantity of speeding, and the pressure of recoil gas tank should be higher than reactor pressure 0.1～1.0Mpa; Need heat the time, the back flushing air body heater places on the pressurized gas inlet pipeline of recoil gas tank at recoil gas, with heat medium gases at high pressure is heated to temperature near reactor.
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| CN102773050A (en) * | 2012-08-14 | 2012-11-14 | 迈瑞尔实验设备（上海）有限公司 | Structure and method for solid-liquid separation and circulation |
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Application publication date: 20050309 Assignee: SHAANXI FUTURE ENERGY CHEMICAL CO.,LTD. Assignor: Shanghai Yankuang Energy Sources Technology Research & Development Co.,Ltd. Contract record no.: 2012310000147 Denomination of invention: Automatic filtering/back purging system liquid and solid separation for in three phase paste state bed reactor Granted publication date: 20051228 License type: Common License Record date: 20120813 |
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Inventor after: Sun Qiwen Inventor after: Zhu Jicheng Inventor after: Geng Jiahuai Inventor after: Wang Xin Inventor after: Chu Hongchun Inventor before: Zhu Jicheng Inventor before: Geng Jiahuai Inventor before: Wang Xin Inventor before: Chu Hongchun |
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