CN102507259B - Method for sampling solid particles in gas-liquid two phases - Google Patents
Method for sampling solid particles in gas-liquid two phases Download PDFInfo
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- CN102507259B CN102507259B CN 201110299473 CN201110299473A CN102507259B CN 102507259 B CN102507259 B CN 102507259B CN 201110299473 CN201110299473 CN 201110299473 CN 201110299473 A CN201110299473 A CN 201110299473A CN 102507259 B CN102507259 B CN 102507259B
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Abstract
The invention relates to a method for sampling solid particles in gas-liquid two phases by a sampling device. The sampling device comprises a sampler (300) having a closed housing to form an inner cavity isolated from the outside, and also having a sample inlet (330) and a sample outlet (340); a vacuumizing system (400) connected with the sampler (300) via a connection port arranged at the housing of the sampler (300); and a filter (310) arranged inside the sampler (300) and at the connection port so that the vacuumizing system (400) communicates with fluid in the inner cavity of the sampler (300) via the filter (310). The method comprises forming a negative pressure inside the sampler (300) by use of the vacuumizing system (400); allowing solid particles to enter the sampler (300) via the sample inlet (330) under the action of pressure difference; and taking out the solid particles from the sampler (300) via the sample outlet (340). The inventive method is highly efficient, accurate and environment-friendly.
Description
Technical field
The invention provides and a kind ofly for relating to a kind of method of sampling of gas-solid two-phase solid particle, relate in particular to the fluidized solid method of sampling, more specifically, relate to the method for sampling of catalyzer in circulating fluid bed reactor.
Background technology
Ethene in low-carbon alkene and propylene are the important basic materials of modern chemistry industry, and the traditional route of preparing ethylene and propylene is by naphtha pyrolysis production.International oil price is high in recent years take the enterprise that oil gas is raw material and causes significant impact China is many, and the relatively abundant and production capacity of methanol of domestic coal resources and excess production capacity are badly in need of development methyl alcohol application market and Downstream Products of Methanol in addition.For these reasons, the low-carbon alkenes such as Methanol ethene, propylene (Methanol to Olefin is called for short MTO) technology is very fast at Chinese development, and megaton (MT) MTO factory has dropped into commercial operation.The MTO technology will realize Coal Chemical Industry and tradition the docking of " petrochemical complex ", and for mainly take at present coal, be that main methanol industry opens wide development space.
The MTO reaction selects circulating fluid bed reactor to be reacted and catalyst regeneration usually, adopts fluidized bed to have following obvious advantage:
(1) due to vigorous exercise and the back-mixing of catalyst granules, make bed temperature even.In addition, fluidized bed catalyst granules used is more much smaller than fixed bed, and the specific surface area of particle is very large, and therefore, heat transfer and mass transfer rate between gas-solid are more much higher than the fixed bed.High these two key characters of the uniformity of temperature profile of bed and rate of heat transfer make fluidized bed easily regulate and maintain needed temperature.This chemical reaction process for the strong heat release of this class of MTO (37～53kJ/mol) is very important, and the local overheating of bed even " is burnt " situation of catalyzer to death thereby avoided.
(2) for the MTO catalytic reaction of heat release, maintain certain bed temperature, must send out heat, this will in bed, place in heat interchanger.Due to the vigorous exercise of catalyst granules in fluidized bed, constantly wash away heat exchanger wall and, make to be unfavorable for the air film attenuation on the wall of heat exchange, thereby improved the heat transfer coefficient of bed to wall.Usually the required heat transfer area in large ten times of left and right of the ratio of heat transfer coefficient fixed bed of fluidized bed exchange hot side, so fluidized bed is also less, and the structure of heat interchanger is also more simply too much than the fixed bed, thereby has saved metal material, has reduced cost.
(3) due to the quasi-liquid characteristic of fluidized catalyst particle, therefore from bed, take out catalyzer or add new catalyzer convenient especially in bed, easily realizing operation serialization and robotization.Because the MTO catalysts can be covered and lose its activity by coke very soon, regeneration in time, a large amount of like this catalyzer takes out (referred to herein as spent agent) from reactor, (referred to herein as regenerant) Returning reactor again after regeneration, this can't realize in fixed bed.
(4) production intensity of fluidized bed is large, and, when treatment capacity is identical, fluidized bed is more much smaller than fixed bed, thereby is convenient to expand the scale of production.
As seen from the above analysis, in time, gather out reclaimable catalyst accurately and efficiently and the regenerated catalyst sample is analyzed, for instruct produce very crucial.
Yet, MTO reclaimable catalyst and the common sample mode of regenerated catalyst are as shown in Figure 1 at present, during sampling, manually directly at thief hatch 130, 230 places drive valve and use Sheng sample bottle 800 dress samples, following some drawback occurred: during (1) sampling, the catalyzer waste is larger, because reaction is to carry out under positive pressure (0-1.0MPa), temperature of reaction very high (400-500 ℃), regeneration temperature (500-700 ℃), the catalyst recirculation amount is very large, when sample in the historical facts or anecdotes border, once open sampling valve, to there be a large amount of catalyzer to leak, be far longer than and need the sample gathered, caused larger waste, (2) caused certain environmental pollution, due to after catalyst grain size thin (major part is tens microns grades) and reaction containing the carbon distribution of a few percent of having an appointment, color is greyish black, the relatively large catalyst granules major part of revealing during sampling directly floats in ambient air, causes certain environmental pollution, (3) bring certain deviation to the representativeness of sampling, owing to directly under atmospheric environment, with containing the sample bottle, from sampling valve, accessing sample, because the reaction-regeneration system internal circulating load is large and a large amount of pumped (conveying) mediums (catalyst transport is with a large amount of gas) are arranged, the atmospheric environment of perhaps sampling has air turbulence will cause gathered sample granularity skewness, there is part granularity relatively fine particle directly to float among atmosphere and can't collect, causing the deviation while analyzing, (4) sampling operation labour intensity is larger, owing to being manual control switch's sampling valve, therefore floating fine grained is caused certain harm in people's suction body.
Visible, efficient, accurate, the eco-friendly new method of sampling that exploitation makes new advances is very necessary.Because the MTO technology is world today's newest fruits, on Sampling techniques owing to not having ready-made method can use for reference also some technological deficiencies.
Summary of the invention
The present invention relates to the method for sampling of solid particle in a kind of gas-solid two-phase, carry out with sampling apparatus,
Sampling apparatus comprises:
(A) sampling thief, have the housing of sealing, forms the inner chamber be hedged off from the outer world, and has sample inlet and sample export;
(B) pumped vacuum systems, be connected with sampling thief by the connector on the housing that is arranged on sampling thief;
(C) filtrator, in the housing of sampling thief, be arranged on the connector place, makes the cavity fluid UNICOM of pumped vacuum systems via filtrator and sampling thief;
The method comprises the following steps:
(a) make in sampling thief to form negative pressure by pumped vacuum systems;
(b) solid particle is entered in sampling thief under the effect of pressure differential via sample inlet;
(c) solid particle in sampling thief takes out via sample export.
Preferably, the bottom of sampling thief is back taper.
Preferably, sampling apparatus further comprises: (D) blowdown system is connected to the top of sampling thief.
Preferably, sampling apparatus further comprises: (E) purging system shares connector with pumped vacuum systems.
Preferably, sampling apparatus further comprises: (F) pressure indication mechanism is connected to the top of sampling thief.
Preferably, sample inlet is arranged on the top of sampling thief; Sample export is arranged on the bottom of sampling thief.
Preferably, further comprise: (G) sample container is connected to sample export.
Preferably, filtrator has spool, and the aperture of spool is 1～200 μ m.
Preferably, the method for sampling of the present invention further comprises:
(d) purge with purging system the solid particle be gathered in filtrator and enter sampling thief;
(e) take out via sample export the solid particle that the purging in sampling thief obtains.
Preferably, the method for sampling of the present invention further comprises:
(f) cycling step (d) and step (e) be not until have solid particle to discharge.
Preferably, the solid particle in sampling thief leaks into sample container under pressure-fired and Action of Gravity Field.
On-line sampling method in the situation that the method for sampling of the present invention is the process units operation.
Preferably, process units accommodates fluidized particles, has thief hatch; Wherein, the thief hatch of process units is connected with the sample inlet of sampling apparatus.
Preferably, process units is selected from fluidized-bed reactor, catalyst regenerator.
Preferably, process units comprises:
(R1) fluidized-bed reactor, have reclaimable catalyst outlet and regenerated catalyst entrance; And
(R2) catalyst regenerator, have reclaimable catalyst entrance and regenerated catalyst outlet;
Wherein, the reclaimable catalyst outlet is connected to the reclaimable catalyst entrance; The regenerated catalyst outlet is connected to the regenerated catalyst entrance;
Wherein, the reclaimable catalyst outlet is provided with the reclaimable catalyst thief hatch; The regenerated catalyst outlet is provided with the regenerated catalyst thief hatch; The sample inlet of sampling apparatus is connected with reclaimable catalyst thief hatch and/or regenerated catalyst thief hatch.
Preferably, described solid particle is fluidized particles.
Preferably, the mean grain size of solid particle≤500 μ m, preferably≤300 μ m, more preferably≤200 μ m, more preferably≤100 μ m also, further preferably≤50 μ m, further preferably≤30 μ m also, most preferably≤10 μ m, particularly preferably≤5 μ m.
The method of sampling of the present invention is efficient, accurate, environmental friendliness.
The accompanying drawing explanation
The sampling apparatus schematic diagram that Fig. 1 is correlation technique.
The schematic diagram of a kind of preferred implementation that Fig. 2 is sampling apparatus of the present invention.
The schematic diagram of a kind of preferred implementation that Fig. 3 is sampling system of the present invention.
Embodiment
In the present invention, " with ... be connected " or " being connected to " or " connection ", can be both that the two directly is connected or is communicated with, also can for example, across common parts or device (valve), be connected or connect or be communicated with.
In the present invention, in the situation that not contradiction or conflict, all embodiment of the present invention, embodiment and feature can combine mutually.
In the present invention, all units, parts etc., both can be purchased, also can be according to content self-control disclosed by the invention.
In the present invention, for outstanding emphasis of the present invention, the omission that operation and unit, the parts of some routines are carried out, or only do simple the description.
In the present invention, identical drawing reference numeral means identical parts or device.
In the present invention, term " reclaimable catalyst " or " spent agent " are the abbreviations for the treatment of regenerated catalyst.
In the present invention, term " regenerated catalyst " or " regenerant " are the abbreviations of the catalyzer after regeneration.
The present invention is directed to the shortcoming of above-mentioned common sampling method, provide a kind of reliable, accurately, sampling apparatus and the method for sampling of catalyzer in efficient, environmental friendliness and the high recirculating fluidized bed of automaticity.
One aspect of the present invention relates to a kind of fluidized particles sampling apparatus sampling apparatus of solid particle (or in the gas-solid two-phase), comprising:
(A) sampling thief, have the housing of sealing, forms the inner chamber be hedged off from the outer world, and has sample inlet and sample export;
(B) pumped vacuum systems, be connected with (A) sampling thief by the connector be arranged on housing;
(C) filtrator, in the housing of (A) sampling thief, be arranged on the connector place, makes the cavity fluid UNICOM of pumped vacuum systems via filtrator and sampling thief.
(A) sampling thief has the housing of sealing, forms the inner chamber be hedged off from the outer world, and has sample inlet and sample export.Preferably, (A) sample inlet of sampling thief is arranged on the top of (A) sampling thief.Preferably, (A) sample export of sampling thief is arranged on the bottom of (A) sampling thief.The sample inlet place can be provided with sampling valve (the first valve).The sample export place can arrange sample export valve (the 3rd valve).
The design of sampling thief shape will consider that gathered catalyst granules easily enters and contains the sample bottle from sampling thief, and for example, certain taper or radian, tapering are arranged at the sampling thief bottom can be 1 °～175 °.Preferably, (A) bottom of sampling thief is back taper.Because the bottom of (A) sampling thief is the downward taper of cone point, like this, the sample of being convenient to enter into (A) sampling thief inner chamber is easy to collect and get rid of by the sample export that is positioned at bottom.
Preferably, (B) pumped vacuum systems is connected to (A) sampling thief.(B) pumped vacuum systems is connected with (A) sampling thief by the connector be arranged on housing.Therefore, (B) pumped vacuum systems via (C) filtrator and (A) the cavity fluid UNICOM of sampling thief.(B) pumped vacuum systems and (A) be provided with valve (second valve) between sampling thief.Pumped vacuum systems is discharged gas in sampling thief, and the vacuum tightness that for example makes (A) sampling thief is 0～-1.01 * 105Pa.
Preferably, (C) filter bits, in the housing of (A) sampling thief, is arranged on (B) pumped vacuum systems and (A) the connector place of sampling thief.(C) filtrator prevents that the fine grained of institute's sample thief from entering vacuum system.For example, filtrator spool aperture is 1～200 μ m.
Preferably, sampling apparatus of the present invention further comprises: (D) blowdown system is connected to (A) sampling thief.(D) blowdown system can with the cavity fluid UNICOM of (A) sampling thief.(D) blowdown system can guarantee the safety of (A) sampling thief.Preferably, (D) blowdown system is connected in the top of (A) sampling thief, for example is connected in the top of (A) sampling thief.
Preferably, sampling apparatus of the present invention further comprises: (E) purging system (or being called blowback system) is connected to (A) sampling thief.Equally, (E) purging system is via (C) filtrator and (A) the cavity fluid UNICOM of sampling thief.Preferably, (E) purging system and (B) pumped vacuum systems share and (A) connector of sampling thief.Like this, (E) purging system just can purge the sample powder be gathered on filtrator.(E) purging system and (A) be provided with valve (the 4th valve) between sampling thief.The purge gas that purging system adopts is the gas without impact on sampling system.Purge gas (blowback medium) can be nitrogen, air, water vapor, indifferent gas or other on sampling system the gas without impact.
Sampling apparatus of the present invention further comprises: (F) pressure indication mechanism is connected to (A) sampling thief.(F) the pressure indication mechanism can with (A) sampling thief fluid communication.(F) the pressure indication mechanism is for showing (A) sampling thief vacuum tightness.Preferably, (F) the pressure indication mechanism is connected in the top of (A) sampling thief, for example is connected in the top of (A) sampling thief.
Sampling apparatus of the present invention further comprises: (G) sample container.(G) sample container is for holding the sample of discharging from sample export.How the Sheng sample bottle size adopted does not limit, and for all holding gathered sample, is purpose.For example, sample container is connected to sample export.As another kind of embodiment, sample container can be independent parts, when using, is connected to sample export, or directly is placed on the sample export below.
Preferably, the particle diameter of solid particle or fluidized particles≤500 μ m, preferably≤300 μ m, more preferably≤200 μ m, more preferably≤100 μ m also, further preferably≤50 μ m, further preferably≤30 μ m also, most preferably≤10 μ m, particularly preferably≤5 μ m.
Preferably, the mean grain size of solid particle or fluidized particles≤500 μ m, preferably≤300 μ m, more preferably≤200 μ m, more preferably≤100 μ m also, further preferably≤50 μ m, further preferably≤30 μ m also, most preferably≤10 μ m, particularly preferably≤5 μ m.
Preferably, fluidized particles is catalyzer.Preferably, catalyzer is molecular sieve catalyst, preferably phosphoric acid Si-Al molecular sieve catalyzer, more preferably SAPO molecular sieve catalyst, most preferably SAPO-34 molecular sieve catalyst.
The invention still further relates to a kind of sampling system, comprising:
Sampling apparatus of the present invention;
Process units, accommodate fluidized particles, has thief hatch;
Wherein, the thief hatch of process units is connected with the sample inlet of sampling apparatus.
Preferably, process units is selected from fluidized-bed reactor, catalyst regenerator.
Preferably, process units comprises:
(R1) fluidized-bed reactor, have reclaimable catalyst outlet and regenerated catalyst entrance; And
(R2) catalyst regenerator, have reclaimable catalyst entrance and regenerated catalyst outlet.
Wherein, the reclaimable catalyst outlet is connected to the reclaimable catalyst entrance; The regenerated catalyst outlet is connected to the regenerated catalyst entrance.
The reclaimable catalyst outlet is provided with the reclaimable catalyst thief hatch; The regenerated catalyst outlet is provided with the regenerated catalyst thief hatch.The sample inlet of sampling apparatus is connected with reclaimable catalyst thief hatch and/or regenerated catalyst thief hatch.Preferably, the sample inlet of sampling apparatus is connected with reclaimable catalyst thief hatch and/or regenerated catalyst thief hatch.
The reclaimable catalyst thief hatch is provided with reclaimable catalyst valve (the 5th valve); The regenerated catalyst thief hatch is provided with regenerated catalyst valve (the 6th valve).
Preferably, accommodate catalyzer in fluidized-bed reactor.Preferred catalyst is silicoaluminophosphamolecular molecular sieve catalyst, more preferably SAPO molecular sieve catalyst, most preferably SAPO-34 molecular sieve catalyst.
Preferably, (R1) fluidized-bed reactor is methanol to olefins reaction device (MTO reactor).
The object of the invention is: provide a kind of reliable, accurately, the sampling apparatus of catalyzer in efficient, environmental friendliness and the high recirculating fluidized bed of automaticity.
For solve artificial directly at the thief hatch place, open valve use contain the bottled sample of sample and occur such as sampling the time catalyzer waste large, cause certain environmental pollution, to the representativeness of sampling, bring the drawbacks such as certain deviation, sampling operation labour intensity are larger, the inventor wishes to make reclaimable catalyst or regenerated catalyst enter sampling thief from thief hatch separately by the switch of operation valve, change to realize that by the pressure in sampling thief the catalyst sample in sampling thief is discharged into Sheng sample bottle again, to reach the sampling purpose.
The invention provides a kind of sampling apparatus for the recirculating fluidized bed reacting middle catalyst, comprise with lower component: (1) one temporary from the reclaimable catalyst of reclaimable catalyst or regenerated catalyst thief hatch or the sampling thief of regenerated catalyst; (2) a set of be connected in sampling thief provide the pumped vacuum systems of subnormal ambient for sampling system; (3) one fine graineds that prevent institute's sample thief that are placed on sampling thief inside enter the filtrator of vacuum system; (4) a set of nitrogen system for power back-blowing filter; (5) a set of sampling thief that is connected in is also for guaranteeing its safe blowdown system; (6) the pressure indication mechanism of a set of demonstration sampling thief pressure; (7) 4 cover switching control pilots, control respectively reclaimable catalyst or regenerated catalyst and enter that sampling thief, nitrogen enter sampling thief, the sampling thief pumped vacuum systems enters Sheng sample bottle with the sample of adopting; (8) Shengs are fetched the Sheng sample bottle from sampling thief sample particle.
The present invention relates to the fluidized particles method of sampling (or being called the method for sampling of solid particle in the gas-solid two-phase or the fluidized particles method of sampling in gas phase) on the other hand.
Preferably, the fluidized particles method of sampling of the present invention adopts fluidized particles sampling apparatus according to the present invention to carry out.
A kind of preferred embodiment in, method of the present invention sampling apparatus of the present invention carries out,
Wherein, sampling apparatus comprises:
(A) sampling thief, have the housing of sealing, forms the inner chamber be hedged off from the outer world, and has sample inlet and sample export;
(B) pumped vacuum systems, be connected with (A) sampling thief by the connector be arranged on housing; And
(C) filtrator, in the housing of (A) sampling thief, be arranged on the connector place, and pumped vacuum systems is via the cavity fluid UNICOM of filtrator and sampling thief;
The method comprises the following steps:
(a) make in sampling thief to form negative pressure by pumped vacuum systems;
(b) solid particle is entered in sampling thief under the effect of pressure differential via sample inlet;
(c) solid particle in sampling thief takes out via sample export.
A kind of preferred embodiment in, method of the present invention comprises:
(a) close sample inlet and sample export, by pumped vacuum systems, make in sampling thief to form negative pressure;
(b) open sample inlet, solid particle is entered in sampling thief via sample inlet under the effect of pressure differential, then close sample inlet;
(c) open sample export, the solid particle in sampling thief takes out via sample export.
Preferably, if sampling apparatus comprises (E) purging system, in step (a), (E) purging system and (A) also close between sampling thief.That is to say, in step (a), (E) purge gas in the purging system can not enter (A) sampling thief.
Preferably, at step (b), solid particle is entered in sampling thief under the effect of pressure differential via sample inlet.Preferably, at step (b), when the sampling thief internal pressure reaches whole system pressure, close sample inlet.In other words, during pressure equilibrium, then close sample inlet.
Preferably, in step (c), the solid particle (material) in sampling thief leaks under pressure-fired and Action of Gravity Field contains the sample bottle.
Preferably, method of the present invention further comprises:
(d) purge with (E) purging system the solid particle be gathered in filtrator, make it enter sampling thief;
(e) take out via sample export the solid particle that the purging in sampling thief obtains.
Preferably, in step (d), purge and to carry out approaching under the condition of reaction pressure.Preferably, in step (e), the solid particle (material) in sampling thief leaks under pressure-fired and Action of Gravity Field contains the sample bottle.
Preferably, method of the present invention further comprises:
(f) cycling step (d) and step (e).
Preferably, in step (f), cycling step (d) and step (e) be not until have solid particle to discharge.
Preferably, method of the present invention is the on-line sampling method of solid particle in the gas-solid two-phase.In the present invention, " on-line sampling method " is from the method for sampling wherein in the situation of process units operation.In this case, fluidized particles refers to that fluidized particles (solid particle in the gas-solid two-phase) is for the fluidized particles in the device of producing.
Preferably, the on-line sampling method in the situation that the method for sampling is the process units operation.
Preferably, the method for sampling of the present invention is undertaken by the above-mentioned sampling system of the present invention.
Preferably, solid particle of the present invention is fluidized particles.
Compare with existing sampling apparatus, the present invention is directed to the shortcoming of existing common sampling apparatus, provide a kind of reliable, accurately, the method for sampling of catalyzer in efficient, environmental friendliness and the high recirculating fluidized bed of automaticity.
Below in conjunction with Fig. 2 of the present invention and Fig. 3, embodiments of the invention are further described.
As shown in Figures 2 and 3, the sampling apparatus of fluidized particles of the present invention comprises: sampling thief 300, pumped vacuum systems 400, filtrator 310.
Sampling thief 300 has the housing of sealing, forms the inner chamber be hedged off from the outer world, and has sample inlet 330 and sample export 340.Sample inlet 330 is arranged on the top of sampling thief 300.Sample export 340 is arranged on the bottom of sampling thief 300.Sample inlet 330 places can be provided with sampling valve (the first valve) 701.Sample export 340 places can arrange sample export valve (the 3rd valve) 703.The bottom of sampling thief 300 is back taper, and the sample of being convenient to enter into sampling thief 300 inner chambers is easy to collect and get rid of by the sample export 340 that is positioned at bottom.Sampling thief 300 volumes will be considered to choose applicable volume size according to combined factors such as sampling quantity, system pressure, solid holdup, operation ease, and for example its volume can be 0.1L～50L.
Pumped vacuum systems 400 is connected to sampling thief 300.Pumped vacuum systems 400 is connected with sampling thief 300 by the connector be arranged on housing.Connector is arranged on the top of sampling thief 300.Be provided with valve (second valve) 702 between pumped vacuum systems 400 and sampling thief 300.
On the inwall of sampling thief 300, be positioned at the connector place, be provided with filtrator 310.Filtrator 310 prevents that the fine grained of institute's sample thief from entering vacuum system 400.Like this, pumped vacuum systems 400 is via the cavity fluid UNICOM of filtrator 310 and sampling thief 300.
This sampling apparatus further comprises: blowdown system 500 is connected to the top of sampling thief 300.Blowdown system 500 can guarantee the safety of sampling thief 300.
This sampling apparatus further comprises: purging system 600 shares the connector with sampling thief 300 with pumped vacuum systems 400.That is, purging system is through the 600 cavity fluid UNICOMs by filtrator 310 and sampling thief 300.As shown in the figure, purging system 600 is connected between second valve 702 and filtrator 310.Like this, purging system 600 just can purge the sample particle be gathered on filtrator 310.Be provided with valve (the 4th valve) 704 between purging system 600 and sampling thief 300.Purging system 600 can adopt inert gas or nitrogen as purge gas.
This sampling apparatus further comprises: pressure indication mechanism 320 is connected to the top of sampling thief 300.Pressure indication mechanism 320 is for example tensimeter.
This sampling apparatus further comprises: sample container 800, and for holding the sample of discharging from sample export 340.
Below the mode of operation of employing device of the present invention and sampling system described.Below explanation be to take to carry out as example for the sampling apparatus of recirculating fluidized bed reacting middle catalyst.
Reclaimable catalyst thief hatch 130 or regenerated catalyst thief hatch 230 are connected with sampling valve (the first valve) 701 through pipeline, and sampling valve 701 is arranged on sample inlet 330 places of sampling thief 300.The inner upper wall surface of sampling thief 300 is equipped with the filtrator 310 that the fine grained that prevents institute's sample thief enters vacuum system 400.Filtrator 310 is connected with the pumped vacuum systems 400 that subnormal ambient is provided for sampling system through valve (second valve) 702.The nitrogen that is useful on power back-blowing filter 310 between valve 702 and filtrator 310 injects wherein after valve 704 is controlled.Sampling thief 300 lower specimen export 340 places and are controlled by valve 703, and institute's collected specimens enters Sheng sample bottle 800 and completes sampling after valve 703.Sampling thief 300 tops are equipped with the pressure indication mechanism (for example tensimeter) 320 that guarantees its safe blowdown system 500 and show sampling thief 300 pressure.Adopt a plurality of valve blocked operations to realize sampling, the switching between valve can be programmed control, can be also to operate manually.
As shown in Figure 3, fluidized-bed reactor 100 has reclaimable catalyst outlet 110 and regenerated catalyst entrance 120.Catalyst regenerator 200 has reclaimable catalyst entrance 220 and regenerated catalyst outlet 210.Reclaimable catalyst outlet 110 is connected to reclaimable catalyst entrance 220; Regenerated catalyst outlet 210 is connected to regenerated catalyst entrance 120.Like this, when needed, catalyzer takes out (referred to herein as reclaimable catalyst or referred to as spent agent) from fluidized-bed reactor 100, and after regeneration, (referred to herein as regenerated catalyst or regenerant) returns to again fluidized-bed reactor 100.
Reclaimable catalyst thief hatch 130 is provided with reclaimable catalyst valve (the 5th valve) 705; Regenerated catalyst thief hatch 230 is provided with regenerated catalyst valve (the 6th valve) 706.
A kind of preferred embodiment in, the invention provides the method for sampling, the especially method of sampling of recirculating fluidized bed reacting middle catalyst of solid particle in the gas-solid two-phase.
A kind of preferred embodiment in, the method for sampling of the present invention comprises the steps:
The first step: shut-off valve 701, cut off the passage that spent agent or regenerant material enter sampling thief; Shut-off valve 703 and valve 704, make the material in sampling thief can not enter Sheng sample bottle, and the nitrogen of blowback sampling thief internal filter must not enter sampler system simultaneously.
Second step: valve opens 702, opens pumped vacuum systems simultaneously, makes the pressure of sampling thief approach vacuum.
The 3rd step: shut-off valve 702, open valve 701, make spent agent or regenerant sample enter sampling thief under pressure differential exists, when the sampling thief internal pressure reaches whole system pressure, shut-off valve 701.
The 4th step: open valve 703 makes material in sampling thief leak into Sheng sample bottle under pressure-fired and Action of Gravity Field.
The 5th step: shut-off valve 703, open valve 704, make and purge nitrogen anti-catalyst fines be gathered in filtrator that purges under approaching the condition of reaction pressure, make fine powder enter sampling thief.
The 6th step: shut-off valve 704, open valve 703, make in sampling thief and to be swept by the nitrogen blowback fine powder obtained and leak under pressure-fired and Action of Gravity Field and contain the sample bottle.
The 7th step: cycling the 5th step and the 6th step, shut-down operation when not having fine powder to discharge, a sampling period finishes.
The 8th step: when gathering next spent agent or regenerant sample, the repetitive operation first step to the seven steps.
With common sampling apparatus, compare, the advantage of sampling apparatus of the present invention and the method for sampling is: (1) sampling degree of accuracy, accuracy is high, and institute's sample thief is representative strong, and there is no the catalyzer waste; (2) sampling time short, improved sampling efficiency; (3) automaticity is high, has alleviated manual working intensity; (4) environmental friendliness, can not cause environmental pollution.
Adopt the method to gather catalyst sample in recirculating fluidized bed, at present, all there is no the pertinent literature report both at home and abroad.
The following examples will further illustrate the example that uses device sampling provided by the present invention, but the present invention is not therefore subject to any restriction.
Embodiment
Put up sampling apparatus as shown in Figure 2,3, sampling thief is selected the volume of 5L.(1) carry out impermeability and detect, the state of test valve 701～valve 704, make each valve all in closed condition; (2) open the valve 705 (the 5th valve) of reclaimable catalyst thief hatch 130, valve opens 702, opens pumped vacuum systems 400 simultaneously, makes the pressure of sampling thief 300 to-0.94 * 10
5pa; (3) shut-off valve 702, and open valve 701 makes the reclaimable catalyst sample enter sampling thief 300 under pressure differential exists, and treat that it is 0.12 * 10 that sampling thief 300 internal pressures reach system pressure
5during Pa, shut-off valve 701; (4) open valve 703, make the interior material of sampling thief 300 leak under pressure-fired and Action of Gravity Field and contain sample bottle 800; (5) shut-off valve 370, open valve 704, make the purge gas nitrogen of purging system 600 approach 0.12 * 10
5under the condition of Pa pressure, the anti-catalyst fines be gathered in filtrator 310 that purges, make fine powder enter sampling thief 300; (6) shut-off valve 704, and open valve 703 makes the interior fine powder obtained of being swept by the nitrogen blowback of sampling thief 300 leak into Sheng sample bottle 800 under pressure-fired and Action of Gravity Field; Cycling (5) step and (6) step 2 times, be shown in shut-down operation while not having fine powder to discharge, and a sampling period finishes.The reclaimable catalyst sample that sampling obtains the 100g left and right, go to detect the indexs such as granularity, carbon distribution.
Above-described embodiment is only the present invention's specific embodiment preferably, and system features of the present invention is not limited to this, any personnel that are familiar with this technology, in field of the present invention, can think easily and variation or modification, all can be encompassed in the scope of the claims of the present invention.
Certainly, the present invention also can have other embodiments, the foregoing is only the preferred embodiment of the present invention, not is used for limiting protection scope of the present invention; Without departing from the spirit of the invention, those of ordinary skills are every makes various corresponding variations and modification according to content of the present invention, all belongs to the protection domain of claim of the present invention.
Claims (22)
1. the method for sampling of solid particle in a gas-solid two-phase, carry out with sampling apparatus,
Described sampling apparatus comprises:
(A) sampling thief (300), have the housing of sealing, forms the inner chamber be hedged off from the outer world, and has sample inlet (330) and sample export (340);
(B) pumped vacuum systems (400), be connected with described sampling thief (300) by the connector on the housing that is arranged on described sampling thief (300);
(C) filtrator (310), in the housing of described sampling thief (300), be arranged on described connector place, makes the cavity fluid UNICOM of described pumped vacuum systems (400) via described filtrator (310) and described sampling thief (300);
The method comprises the following steps:
(a) make in described sampling thief (300) to form negative pressure by described pumped vacuum systems (400);
(b) solid particle is entered in described sampling thief (300) under the effect of pressure differential via described sample inlet (330);
(c) solid particle in described sampling thief (300) takes out via described sample export (340);
Described sampling apparatus further comprises: (E) purging system (600) shares described connector with described pumped vacuum systems (400);
In described gas-solid two-phase, the method for sampling of solid particle further comprises:
(d) purge with described purging system (600) solid particle be gathered in described filtrator (310) and enter described sampling thief (300);
(e) take out via described sample export (330) solid particle that the purging in described sampling thief (300) obtains.
2. the method for sampling according to claim 1, is characterized in that, the bottom of described sampling thief (300) is back taper.
3. the method for sampling according to claim 1, is characterized in that, described sampling apparatus further comprises: (D) blowdown system (500) is connected to the top of described sampling thief (300).
4. the method for sampling according to claim 1, is characterized in that, described sampling apparatus further comprises: (F) pressure indication mechanism (320) is connected to the top of described sampling thief (300).
5. the method for sampling according to claim 1, is characterized in that, described sample inlet (330) is arranged on the top of described sampling thief (300); Described sample export (340) is arranged on the bottom of described sampling thief (300).
6. the method for sampling according to claim 1, is characterized in that, described sampling apparatus further comprises: (G) sample container (800) is connected to described sample export (340).
7. the method for sampling according to claim 1, is characterized in that, described filtrator (310) has spool, and the aperture of described spool is 1～200 μ m.
8. the method for sampling according to claim 1, is characterized in that, further comprises:
(f) cycling step (d) and step (e) be not until have solid particle to discharge.
9. the method for sampling according to claim 6, is characterized in that, the solid particle in described sampling thief (300) leaks into described sample container (800) under pressure-fired and Action of Gravity Field.
10. according to the described method of sampling of claim 1 to 9 any one, it is characterized in that the on-line sampling method in the situation that the described method of sampling is the process units operation.
11. the method for sampling according to claim 10, is characterized in that,
Described process units accommodates fluidized particles, has thief hatch;
Wherein, the thief hatch of described process units is connected with the sample inlet (330) of described sampling apparatus.
12. the method for sampling according to claim 11, is characterized in that, described process units is selected from fluidized-bed reactor and catalyst regenerator.
13. the method for sampling according to claim 12, is characterized in that, described process units comprises:
(R1) fluidized-bed reactor (100), have reclaimable catalyst outlet (110) and regenerated catalyst entrance (120); And
(R2) catalyst regenerator (200), have reclaimable catalyst entrance (220) and regenerated catalyst outlet (210);
Wherein, described reclaimable catalyst outlet (110) is connected to described reclaimable catalyst entrance (220); Described regenerated catalyst outlet (210) is connected to described regenerated catalyst entrance (120);
Wherein, described reclaimable catalyst outlet (110) is provided with reclaimable catalyst thief hatch (130); Regenerated catalyst outlet (210) is provided with regenerated catalyst thief hatch (230); The sample inlet of described sampling apparatus (330) is connected with described reclaimable catalyst thief hatch (130) and/or described regenerated catalyst thief hatch (230).
14. according to the described method of sampling of claim 1 to 9 any one, it is characterized in that, described solid particle is fluidized particles.
15. according to the described method of sampling of claim 1 to 9 any one, it is characterized in that the mean grain size of described solid particle≤500 μ m.
16. the method for sampling according to claim 15, is characterized in that, the mean grain size of described solid particle≤300 μ m.
17. the method for sampling according to claim 16, is characterized in that, the mean grain size of described solid particle≤200 μ m.
18. the method for sampling according to claim 17, is characterized in that, the mean grain size of described solid particle≤100 μ m.
19. the method for sampling according to claim 18, is characterized in that, the mean grain size of described solid particle≤50 μ m.
20. the method for sampling according to claim 19, is characterized in that, the mean grain size of described solid particle≤30 μ m.
21. the method for sampling according to claim 20, is characterized in that, the mean grain size of described solid particle≤10 μ m.
22. the method for sampling according to claim 21, is characterized in that, the mean grain size of described solid particle≤5 μ m.
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| WO2017105786A1 (en) * | 2015-12-16 | 2017-06-22 | Uop Llc | Method and apparatus for catalyst sampling |
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| CN103674627B (en) * | 2013-12-13 | 2016-06-08 | 神华集团有限责任公司 | The acquisition method of gas/vapour mixture |
| CN109126641B (en) * | 2017-06-15 | 2022-03-01 | 国家能源投资集团有限责任公司 | Fischer-Tropsch synthesis catalyst fluidized bed reduction device and online sampling method |
| CN108489773B (en) * | 2018-03-14 | 2020-10-09 | 中国科学院过程工程研究所 | Sample collection device, system, method and storage medium |
| CN111721599B (en) * | 2020-06-23 | 2021-08-27 | 南京大学 | Atomic-level material beam variable-temperature liquid coating collection method and device in vacuum |
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