CN102507259A - 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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- CN102507259A CN102507259A CN2011102994732A CN201110299473A CN102507259A CN 102507259 A CN102507259 A CN 102507259A CN 2011102994732 A CN2011102994732 A CN 2011102994732A CN 201110299473 A CN201110299473 A CN 201110299473A CN 102507259 A CN102507259 A CN 102507259A
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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 a kind of a kind of gas-solid two method of sampling of solid particle mutually that is used for relating to, relate in particular to the fluidized solid method of sampling, more specifically, relate to the method for sampling of catalyzer in the circulating fluid bed reactor.
Background technology
Ethene in the low-carbon alkene and propylene are the important basic materials of modern chemistry industry, and the traditional route of producing ethene and propylene is through naphtha pyrolysis production.In recent years international oil price high many to China be that the enterprise of raw material causes significant impact with oil gas, the abundant relatively and production capacity of methanol of domestic in addition coal resources is badly in need of developing methyl alcohol application market and Downstream Products of Methanol with excess production capacity.For these reasons, low-carbon alkenes such as methyl alcohol system 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 ", for main at present be that main methanol industry opens wide development space with the coal.
The MTO reaction selects for use circulating fluid bed reactor to react and catalyst regeneration usually, adopts fluidized bed to have following obvious advantage:
(1) because the vigorous exercise and the back-mixing of catalyst granules make bed temperature even.In addition, the used catalyst granules of fluidized bed is much littler than fixed bed, and the specific surface area of particle is very big, 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 regulate and keep needed temperature easily.(37～53kJ/mol) chemical reaction process is crucial, the situation of the local overheating of bed even " burning to death " catalyzer thereby be able to avoid for the strong heat release of this type of MTO for this.
(2) for the MTO catalytic reaction of heat release, keep certain bed temperature, must send out heat, heat interchanger in this will place in bed.Because the vigorous exercise of catalyst granules in the fluidized bed, constantly wash away heat exchanger wall and, make the air film attenuation on the wall that is unfavorable for heat exchange, thereby improved the heat transfer coefficient of bed wall.Usually the heat transfer coefficient of fluidized bed exchange hot side is than about big ten times of fixed bed, so the required heat transfer area of fluidized bed is also less, and also much simple than fixed bed of the structure of heat interchanger, thereby practiced thrift metal material, reduced cost.
(3) because the quasi-liquid characteristic of fluidized catalyst particle, it is convenient especially therefore from bed, to take out catalyzer or in bed, add new catalyzer, realizes operation serialization and robotization easily.Owing to can being covered by coke very soon, the MTO catalysts loses its activity; Regeneration in time; A large amount of like this catalyzer takes out (being called spent agent here) from reactor, (being called regenerant here) Returning reactor again after regeneration, and this can't realize in fixed bed.
(4) production intensity of fluidized bed is big, and promptly when treatment capacity was identical, fluidized bed was much littler than fixed bed, thereby was convenient to expand the scale of production.
Visible by above-mentioned 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; Manual work is directly driven valve and use to be contained appearance bottle 800 dress appearance at thief hatch 130,230 places, some drawback below having occurred: during (1) sampling the catalyzer waste bigger because reaction is to carry out (0-1.0MPa) under positive pressure; Temperature of reaction very high (400-500 ℃), regeneration temperature (500-700 ℃), the catalyst recirculation amount is very big; When sample in the historical facts or anecdotes border,, will there be a large amount of catalyzer to leak in case open sampling valve; Be far longer than the sample that needs collection, caused bigger waste; (2) caused certain environmental pollution; Owing to contain the carbon distribution of a few percent of having an appointment after catalyst grain size thin (major part is tens microns grades) and the reaction; Color is greyish black; More a large amount of catalyst granules major part of revealing during sampling directly floats in the ambient air, causes certain environmental pollution; (3) bring certain deviation for the representativeness of sampling; Owing to directly under atmospheric environment, access sample from sampling valve with containing the appearance bottle; Because the reaction-regeneration system internal circulating load is big and a large amount of pumped (conveying) mediums (catalyst transport has a large amount of gases) are arranged; The atmospheric environment of perhaps sampling has air turbulence will cause the sample granularity skewness of being gathered, and promptly has the part granularity directly to float among the atmosphere than fine grained and can't collect, and causes the deviation when analyzing; (4) sampling operation labour intensity is bigger, owing to be manual control switch's sampling valve, so floating fine grained is caused certain harm in people's suction body.
It is thus clear that 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, also there are not some technological deficiencies owing to there is ready-made method to use for reference.
Summary of the invention
The present invention relates to the method for sampling of solid particle in a kind of gas-solid two mutually, carry out with sampling apparatus,
Sampling apparatus comprises:
(A) sampling thief has the housing of sealing, forms the inner chamber that is hedged off from the outer world, and has sample inlet and sample export;
(B) pumped vacuum systems links to each other with sampling thief through the connector on the housing that is arranged on sampling thief;
(C) filtrator in the housing of sampling thief, is arranged on the connector place, makes the cavity fluid UNICOM of pumped vacuum systems via filtrator and sampling thief;
This method may further comprise the steps:
(a) make with pumped vacuum systems and form negative pressure in the sampling thief;
(b) solid particle is got in the sampling thief under action of pressure via sample inlet;
(c) solid particle in the sampling thief takes out via sample export.
Preferably, the bottom of sampling thief is a 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, and with the shared connector of 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 the solid particle that accumulates in the filtrator with purging system and get into sampling thief;
(e) take out the solid particle that the purging in the sampling thief obtains via sample export.
Preferably, the method for sampling of the present invention further comprises:
(f) cycling step (d) and step (e) are up to there not being solid particle to discharge.
Preferably, the solid particle in the sampling thief leaks into sample container under pressure-fired and action of gravity.
The method of sampling of the present invention is the on-line sampling method under the situation of process units operation.
Preferably, process units accommodates fluidized particles, has thief hatch; Wherein, the thief hatch of process units links to each other 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 has reclaimable catalyst outlet and regenerated catalyst inlet; And
(R2) catalyst regenerator has reclaimable catalyst inlet and regenerated catalyst outlet;
Wherein, the reclaimable catalyst outlet is connected to the reclaimable catalyst inlet; The regenerated catalyst outlet is connected to the regenerated catalyst inlet;
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 links to each other with reclaimable catalyst thief hatch and/or regenerated catalyst thief hatch.
Preferably, said solid particle is a fluidized particles.
Preferably, the mean grain size of solid particle≤500 μ m, preferably≤300 μ m, more preferably≤200 μ m, also more preferably≤100 μ m, further preferred≤50 μ m, also preferably further≤30 μ m, most preferably≤10 μ m, preferred≤5 μ m especially.
The method of sampling of the present invention is efficient, accurate, environmental friendliness.
Description of drawings
Fig. 1 is the sampling apparatus synoptic diagram of correlation technique.
Fig. 2 is the synoptic diagram of a kind of preferred implementation of sampling apparatus of the present invention.
Fig. 3 is the synoptic diagram of a kind of preferred implementation of sampling system of the present invention.
Embodiment
In the present invention, " with ... link to each other " or " being connected to " or " connections ", both can be that the two directly links to each other or is communicated with, also can link to each other or connect or connection across common parts or device (for example valve).
In the present invention, under the situation of not contradiction or conflict, all embodiment of the present invention, embodiment and characteristic can make up each other.
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 some conventional operations and unit, parts are carried out, or only do simple description.
In the present invention, identical drawing reference numeral is represented identical parts or device.
In the present invention, term " reclaimable catalyst " or " spent agent " are the abbreviations of treating regenerated catalyst.
In the present invention, term " regenerated catalyst " or " regenerant " are the abbreviations of the catalyzer after the regeneration.
The present invention is directed to the shortcoming of above-mentioned common sampling method, provide a kind of reliable, accurately, the sampling apparatus and the method for sampling of catalyzer in the high recirculating fluidized bed of efficient, environmental friendliness and automaticity.
One aspect of the present invention relates to a kind of fluidized particles sampling apparatus (or in the gas-solid two mutually the sampling apparatus of solid particle), comprising:
(A) sampling thief has the housing of sealing, forms the inner chamber that is hedged off from the outer world, and has sample inlet and sample export;
(B) pumped vacuum systems links to each other with (A) sampling thief through the connector that is arranged on the housing;
(C) filtrator in the housing of (A) sampling thief, is 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 that is 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 (first valve).The sample export place can be provided with sample export valve (the 3rd valve).
The sampling thief shaped design to consider the catalyst granules of gathering enter from sampling thief easily and contain the appearance bottle, 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 a back taper.Because (A) bottom of sampling thief is the downward taper of awl point, like this, the sample of being convenient to enter into (A) sampling thief inner chamber is easy to collect and get rid of through the sample export that is positioned at the bottom.
Preferably, (B) pumped vacuum systems is connected to (A) sampling thief.(B) pumped vacuum systems links to each other with (A) sampling thief through the connector that is arranged on the 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 the sampling thief.Pumped vacuum systems is discharged gas in the sampling thief, and the vacuum tightness that for example makes (A) sampling thief is 0～-1.01 * 105Pa.
Preferably, (C) filter bits is arranged on (B) pumped vacuum systems and (A) the connector place of sampling thief in the housing of (A) sampling thief.(C) filtrator prevents that the fine grained of institute's sample thief from getting into 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 shared with (A) connector of sampling thief.Like this, (E) purging system just can purge the sample powder that accumulates on the filtrator.(E) purging system and (A) be provided with valve (the 4th valve) between the sampling thief.The purge gas that purging system adopted is not for there being the gas of influence to sampling system.Purge gas (blowback medium) can be that nitrogen, air, water vapor, indifferent gas or other do not have the gas of influence to sampling system.
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 used 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 used to hold the sample of discharging from sample export.How the Sheng appearance bottle size that adopts does not limit, and is purpose for all holding the sample of being gathered.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, perhaps 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, also more preferably≤100 μ m, further preferred≤50 μ m, also preferably further≤30 μ m, most preferably≤10 μ m, preferred≤5 μ m especially.
Preferably, the mean grain size of solid particle or fluidized particles≤500 μ m, preferably≤300 μ m, more preferably≤200 μ m, also more preferably≤100 μ m, further preferred≤50 μ m, also preferably further≤30 μ m, most preferably≤10 μ m, preferred≤5 μ m especially.
Preferably, fluidized particles is a catalyzer.Preferably, catalyzer is a 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 accommodates fluidized particles, has thief hatch;
Wherein, the thief hatch of process units links to each other 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 has reclaimable catalyst outlet and regenerated catalyst inlet; And
(R2) catalyst regenerator has reclaimable catalyst inlet and regenerated catalyst outlet.
Wherein, the reclaimable catalyst outlet is connected to the reclaimable catalyst inlet; The regenerated catalyst outlet is connected to the regenerated catalyst inlet.
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 links to each other with reclaimable catalyst thief hatch and/or regenerated catalyst thief hatch.Preferably, the sample inlet of sampling apparatus links to each other 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 the fluidized-bed reactor.Preferred catalyst is the silicoaluminophosphamolecular molecular sieves catalyzer, more preferably SAPO molecular sieve catalyst, most preferably SAPO-34 molecular sieve catalyst.
Preferably, (R1) fluidized-bed reactor is methanol to olefins reaction device (a MTO reactor).
The object of the invention is: provide a kind of reliable, accurately, the sampling apparatus of catalyzer in the high recirculating fluidized bed of efficient, environmental friendliness and automaticity.
For solve artificial directly open at the thief hatch place valve use contain the bottled appearance of appearance and occur such as sampling the time catalyzer waste big, cause certain environmental pollution, bring drawbacks such as certain deviation, sampling operation labour intensity are bigger for the representativeness of sampling; The inventor hopes that the switch through operation valve makes reclaimable catalyst or regenerated catalyst get into sampling thief from separately thief hatch; Change the catalyst sample of realizing in the sampling thief through the pressure in the sampling thief again and be discharged into Sheng appearance bottle, to reach the sampling purpose.
The invention provides a kind of sampling apparatus that is used 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; What (2) one covers were connected in sampling thief provides the pumped vacuum systems of subnormal ambient for sampling system; (3) one are placed on the inner fine grained that prevents institute's sample thief of sampling thief gets into the filtrator of vacuum system; (4) one covers are used for the nitrogen system of blowback filtrator; (5) one covers are connected in sampling thief and are its safe blowdown system of assurance; (6) one covers show the pressure indication mechanism of sampling thief pressure; (7) 4 overlap switching control pilots, control reclaimable catalyst or regenerated catalyst entering sampling thief, nitrogen entering sampling thief, sampling thief pumped vacuum systems and the institute's sample of adopting entering Sheng kind bottle respectively; (8) Shengs are fetched the Sheng appearance bottle from sampling thief sample particle.
The present invention relates to the fluidized particles method of sampling method of sampling or the fluidized particles method of sampling in the gas phase of solid particle in the gas-solid two mutually (or be called) 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 has the housing of sealing, forms the inner chamber that is hedged off from the outer world, and has sample inlet and sample export;
(B) pumped vacuum systems links to each other with (A) sampling thief through the connector that is arranged on the housing; And
(C) filtrator in the housing of (A) sampling thief, is arranged on the connector place, and pumped vacuum systems is via the cavity fluid UNICOM of filtrator and sampling thief;
This method may further comprise the steps:
(a) make with pumped vacuum systems and form negative pressure in the sampling thief;
(b) solid particle is got in the sampling thief under action of pressure via sample inlet;
(c) solid particle in the 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, make with pumped vacuum systems to form negative pressure in the sampling thief;
(b) open sample inlet, solid particle is got in the sampling thief via sample inlet under action of pressure, close sample inlet then;
(c) open sample export, the solid particle in the sampling thief takes out via sample export.
Preferably, if sampling apparatus comprises (E) purging system, then in step (a), (E) purging system and (A) also close between the sampling thief.That is to say that in step (a), (E) purge gas in the purging system can not get into (A) sampling thief.
Preferably, at step (b), solid particle is got in the sampling thief under action of pressure via sample inlet.Preferably, at step (b), when treating that the sampling thief internal pressure reaches total system pressure, close sample inlet.In other words, during pressure equilibrium, close sample inlet again.
Preferably, in step (c), the solid particle (material) in the sampling thief leaks under pressure-fired and action of gravity contains the appearance bottle.
Preferably, method of the present invention further comprises:
(d) purge the solid particle that accumulates in the filtrator with (E) purging system, make it get into sampling thief;
(e) take out the solid particle that the purging in the sampling thief obtains via sample export.
Preferably, in step (d), purge and under near the condition of reaction pressure, carry out.Preferably, in step (e), the solid particle (material) in the sampling thief leaks under pressure-fired and action of gravity contains the appearance 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) are up to there not being solid particle to discharge.
Preferably, method of the present invention is the on-line sampling method of solid particle in the gas-solid two mutually.In the present invention, " on-line sampling method " is from the method for sampling wherein under the situation of process units operation.In this case, fluidized particles refers to that fluidized particles (solid particle in the gas-solid two mutually) is the fluidized particles in the device of producing.
Preferably, the method for sampling is the on-line sampling method under the situation of process units operation.
Preferably, the method for sampling of the present invention is carried out through the above-mentioned sampling system of the present invention.
Preferably, solid particle of the present invention is a 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 the high recirculating fluidized bed of efficient, environmental friendliness and 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 that is 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 (first valve) 701.Sample export 340 places can be provided with sample export valve (the 3rd valve) 703.The bottom of sampling thief 300 is a back taper, and the sample of being convenient to enter into sampling thief 300 inner chambers is easy to collect and get rid of through the sample export 340 that is positioned at the bottom.Sampling thief 300 volumes will be considered to choose suitable 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 links to each other with sampling thief 300 through the connector that is arranged on the housing.Connector is arranged on the top of sampling thief 300.Be provided with valve (second valve) 702 between pumped vacuum systems 400 and the 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 getting into vacuum system 400.Like this, pumped vacuum systems 400 is via the cavity fluid UNICOM of filtrator 310 with 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, the connector of and sampling thief 300 shared 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 the filtrator 310.Like this, purging system 600 just can purge the sample particle that accumulates on the filtrator 310.Be provided with valve (the 4th valve) 704 between purging system 600 and the 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 for example is a tensimeter.
This sampling apparatus further comprises: sample container 800 is used to hold the sample of discharging from sample export 340.
Mode of operation in the face of employing device of the present invention and sampling system describes down.Below explanation be to be that example is carried out with the sampling apparatus that is used for the recirculating fluidized bed reacting middle catalyst.
Reclaimable catalyst thief hatch 130 or regenerated catalyst thief hatch 230 link to each other with sampling valve (first valve) 701 through pipeline, and sampling valve 701 is installed in sample inlet 330 places of sampling thief 300.Sampling thief 300 inner upper wall surfaces are equipped with the fine grained that prevents institute's sample thief and get into the filtrator 310 of 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 blowback filtrator 310 between valve 702 and the filtrator 310 injects wherein after valve 704 controls.Sampling thief 300 lower specimen export 340 places by valve 703 controls, and institute's collected specimens gets into Sheng appearance bottle 800 through valve 703 backs and accomplishes sampling.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 the valve can be programmed control, also can be to operate manually.
As shown in Figure 3, fluidized-bed reactor 100 has reclaimable catalyst outlet 110 and regenerated catalyst inlet 120.Catalyst regenerator 200 has reclaimable catalyst inlet 220 and regenerated catalyst outlet 210.Reclaimable catalyst outlet 110 is connected to reclaimable catalyst inlet 220; Regenerated catalyst outlet 210 is connected to regenerated catalyst inlet 120.Like this, when needs, catalyzer takes out (be called reclaimable catalyst here or abbreviate spent agent as) from fluidized-bed reactor 100, through regeneration after (being called regenerated catalyst or regenerant here) return fluidized-bed reactor 100 again.
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 present 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 mutually.
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 get into sampling thief; Shut-off valve 703 and valve 704 make that the material in the sampling thief can not get into Sheng appearance bottle, and the nitrogen of blowback sampling thief internal filter must not get into sampler system simultaneously.
Second step: opening of valves 702, open pumped vacuum systems simultaneously, make the pressure of sampling thief near vacuum.
The 3rd step: shut-off valve 702, open valve 701 makes spent agent or regenerant sample entering sampling thief in the presence of pressure differential, when treating that the sampling thief internal pressure reaches total system pressure, shut-off valve 701.
The 4th step: open valve 703 makes the interior material of sampling thief under pressure-fired and action of gravity, leak into and contains the appearance bottle.
The 5th step: shut-off valve 703, open valve 704, make to purge nitrogen anti-catalyst fines that accumulates in the filtrator that purges under condition near reaction pressure, make fine powder get into sampling thief.
The 6th step: shut-off valve 704, open valve 703 makes in the sampling thief that being swept the fine powder that obtains by the nitrogen blowback leaks into and contain the appearance bottle under pressure-fired and action of gravity.
The 7th step: the 5th step of cycling and the 6th step, shut-down operation when waiting not have fine powder to discharge, a sampling period finishes.
The 8th step: when gathering next spent agent or regenerant sample, seven steps of the repetitive operation first step to the.
Compare with common sampling apparatus, the advantage of the sampling apparatus of the present invention and the method for sampling is: (1) sampling degree of accuracy, accuracy height, and institute's sample thief is representative strong, and does not have the catalyzer waste; (2) the sampling time weak point has 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 the recirculating fluidized bed, at present, all do not have the pertinent literature report both at home and abroad.
Following embodiment will further specify the instance that uses device sampling provided by the present invention, but therefore the present invention does not receive any restriction.
Embodiment
Put up like Fig. 2, the sampling apparatus shown in 3, sampling thief is selected the volume of 5L for use.(1) carry out impermeability and detect, the state of test valve 701～valve 704 makes each valve all be in closed condition; (2) open the valve 705 (the 5th valve) of reclaimable catalyst thief hatch 130, opening of valves 702 is opened 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 reclaimable catalyst sample entering sampling thief 300 in the presence of pressure differential, treat that sampling thief 300 internal pressures reach system pressure promptly 0.12 * 10
5During Pa, shut-off valve 701; (4) open valve 703, make sampling thief 300 interior materials under pressure-fired and action of gravity, leak into and contain appearance bottle 800; (5) shut-off valve 370, open valve 704, make the purge gas nitrogen of purging system 600 near 0.12 * 10
5The anti-catalyst fines that accumulates in the filtrator 310 that purges makes fine powder get into sampling thief 300 under the condition of Pa pressure; (6) shut-off valve 704, and open valve 703 makes in the sampling thief 300 that being swept the fine powder that obtains by the nitrogen blowback leaks into and contain appearance bottle 800 under pressure-fired and action of gravity; (5) step of cycling and (6) step 2 times, see shut-down operation when not having fine powder to discharge, a sampling period finishes.Sampling obtains the reclaimable catalyst sample about 100g, goes to detect indexs such as granularity, carbon distribution.
The foregoing description is merely the preferable specific embodiment of the present invention, 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 claim of the present invention.
Certainly, the present invention also can have other embodiments, and the above is merely preferred implementation of the present invention, is not to be used for limiting protection scope of the present invention; Under the situation that does not deviate from spirit of the present invention, those of ordinary skills are every to make 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 (17)
1. the method for sampling of solid particle in gas-solid two is mutually carried out with sampling apparatus,
Said sampling apparatus comprises:
(A) sampling thief (300) has the housing of sealing, forms the inner chamber that is hedged off from the outer world, and has sample inlet (330) and sample export (340);
(B) pumped vacuum systems (400) links to each other with said sampling thief (300) through the connector on the housing that is arranged on said sampling thief (300);
(C) filtrator (310) in the housing of said sampling thief (300), is arranged on said connector place, makes said pumped vacuum systems (400) via the cavity fluid UNICOM of said filtrator (310) with said sampling thief (300);
This method may further comprise the steps:
(a) make formation negative pressure in the said sampling thief (300) with said pumped vacuum systems (400);
(b) solid particle is got in the said sampling thief (300) under action of pressure via said sample inlet (330);
(c) solid particle in the said sampling thief (300) takes out via said sample export (340).
2. the method for sampling according to claim 1 is characterized in that, the bottom of said sampling thief (300) is a back taper.
3. the method for sampling according to claim 1 is characterized in that, said sampling apparatus further comprises: (D) blowdown system (500) is connected to the top of said sampling thief (300).
4. the method for sampling according to claim 1 is characterized in that, said sampling apparatus further comprises: (E) purging system (600), and with the shared said connector of said pumped vacuum systems (400).
5. the method for sampling according to claim 1 is characterized in that, said sampling apparatus further comprises: (F) pressure indication mechanism (320) is connected to the top of said sampling thief (300).
6. the method for sampling according to claim 1 is characterized in that, said sample inlet (330) is arranged on the top of said sampling thief (300); Said sample export (340) is arranged on the bottom of said sampling thief (300).
7. the method for sampling according to claim 1 is characterized in that, said sampling apparatus further comprises: (G) sample container (800) is connected to said sample export (340).
8. the method for sampling according to claim 1 is characterized in that, said filtrator (310) has spool, and the aperture of said spool is 1～200 μ m.
9. the method for sampling according to claim 4 is characterized in that, further comprises:
(d) purge the solid particle that accumulates in the said filtrator (310) with said purging system (600) and get into said sampling thief (300);
(e) take out the solid particle that the purging in the said sampling thief (300) obtains via said sample export (330).
10. the method for sampling according to claim 9 is characterized in that, further comprises:
(f) cycling step (d) and step (e) are up to there not being solid particle to discharge.
11. the method for sampling according to claim 7 is characterized in that, the solid particle in the said sampling thief (300) leaks into said sample container (800) under pressure-fired and action of gravity.
12., it is characterized in that the said method of sampling is the on-line sampling method under the situation of process units operation according to each described method of sampling of claim 1 to 11.
13. the method for sampling according to claim 12 is characterized in that,
Said process units accommodates fluidized particles, has thief hatch;
Wherein, the thief hatch of said process units links to each other with the sample inlet (330) of said sampling apparatus.
14. the method for sampling according to claim 13 is characterized in that, said process units is selected from fluidized-bed reactor and catalyst regenerator.
15. the method for sampling according to claim 14 is characterized in that, said process units comprises:
(R1) fluidized-bed reactor (100) has reclaimable catalyst outlet (110) and regenerated catalyst inlet (120); And
(R2) catalyst regenerator (200) has reclaimable catalyst inlet (220) and regenerated catalyst outlet (210);
Wherein, said reclaimable catalyst outlet (110) is connected to said reclaimable catalyst inlet (220); Said regenerated catalyst outlet (210) is connected to said regenerated catalyst inlet (120);
Wherein, said 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 said sampling apparatus (330) links to each other with said reclaimable catalyst thief hatch (130) and/or said regenerated catalyst thief hatch (230).
16., it is characterized in that said solid particle is a fluidized particles according to each described method of sampling of claim 1 to 11.
17., it is characterized in that the mean grain size of said solid particle≤500 μ m according to each described method of sampling of claim 1 to 11; Preferably≤300 μ m, more preferably≤200 μ m, also more preferably≤100 μ m; Further preferably≤50 μ m; Also further preferably≤30 μ m, most preferably≤10 μ m, preferred≤5 μ m especially.
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| CN109126641A (en) * | 2017-06-15 | 2019-01-04 | 神华集团有限责任公司 | Fischer-tropsch synthetic catalyst fluid bed reduction device and on-line period method |
| CN111721599A (en) * | 2020-06-23 | 2020-09-29 | 南京大学 | Atomic-level material beam variable-temperature liquid coating collection method and device in vacuum |
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| 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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