CN108871838A - On-line period device and on-line period method - Google Patents
On-line period device and on-line period method Download PDFInfo
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- CN108871838A CN108871838A CN201710339229.1A CN201710339229A CN108871838A CN 108871838 A CN108871838 A CN 108871838A CN 201710339229 A CN201710339229 A CN 201710339229A CN 108871838 A CN108871838 A CN 108871838A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/18—Devices for withdrawing samples in the liquid or fluent state with provision for splitting samples into portions
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2205—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with filters
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2226—Sampling from a closed space, e.g. food package, head space
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N2001/1031—Sampling from special places
- G01N2001/105—Sampling from special places from high-pressure reactors or lines
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2226—Sampling from a closed space, e.g. food package, head space
- G01N2001/2238—Sampling from a closed space, e.g. food package, head space the gas being compressed or pressurized
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Abstract
The present invention discloses a kind of on-line period device, including：First sampling jar (1), first sampling jar receive the mixing sample exported from high-temperature high-voltage reaction device, will mix sample and be separated into hot phase sample, solid phase sample and hot liquid phase sample；And second sampling jar (2), second sampling jar receive the hot phase sample exported from the first sampling jar, hot phase sample are separated into gas phase sample and cold liquid phase sample.Invention additionally discloses a kind of on-line period methods.The present invention can safely, effectively complete the on-line period to high-temperature high-voltage reaction device, while realize efficiently separating for different phase in sample.
Description
Technical field
The present invention relates to coal chemical technologies, more particularly to on-line period device and on-line period method.
Background technique
F- T synthesis is the important channel of coal clean conversion, and syrup state bed Fischer Tropsch synthesis technology takes hot good, production capacity because of it
High advantage has been increasingly becoming the prevailing technology of F- T synthesis.It is the state of gas, liquid, solid three-phase coexistence in paste state bed reactor,
Wherein gas is mainly CO, CO2、H2、H2O and lower carbon number hydrocarbons, liquid are mainly heavy wax, and solid is micron-sized catalyst granules.
In device operation process, on-line period analysis is carried out by, liquid product gentle to slurry bed system internal accelerator, it will be appreciated that take
The physicochemical property of catalyst and the distribution of product in synthetic reaction process are held in the palm, and instructs the long-term operation of commercial plant
Deng being of great significance.Since sampling operation operating condition is high temperature and pressure, gas is inflammable and explosive and toxic in reactor, reaction
Liquid product Fischer-Tropsch wax easily frozen plug pipeline in sampling process, therefore sampling method in the prior art is difficult to realize pacify
Entirely, stablize, be readily achieved sampling.
Summary of the invention
The object of the present invention is to provide a kind of device and method of on-line period, which can be safely, effectively
Ground is completed to the on-line period of high-temperature high-voltage reaction device, while realizing efficiently separating for different phase in sample.
To achieve the goals above, one aspect of the present invention provides a kind of on-line period device, including：First sampling jar, should
First sampling jar receives the mixing sample exported from high-temperature high-voltage reaction device, and the mixing sample is separated into hot phase sample
Product, solid phase sample and hot liquid phase sample；And second sampling jar, which receives exports from first sampling jar
The hot phase sample is separated into gas phase sample and cold liquid phase sample by the hot phase sample.
Preferably, it is provided with filter in first sampling jar, by the solid phase sample and the hot liquid phase sample
Mutually separate.
Preferably, first sampling jar includes detachably connected top tank and bottom tank, and the filter is that setting exists
Filter septum between the top tank and bottom tank.
Preferably, the edge of the top tank is provided with first flange, and the edge of the bottom tank is provided with second flange, described
The edge of filter septum is clamped between the first flange and the second flange.
Preferably, the central area of the filter septum is provided with filter screen；The filter screen is wire mesh, the mistake
The filtering accuracy of strainer is 25 microns to 45 microns.
Preferably, the intake pipeline of first sampling jar, the outside of first sampling jar and selectivity is described
The export pipeline of first sampling jar is equipped with heating member.
Preferably, the outside of the intake pipeline of second sampling jar and/or second sampling jar are equipped with cooling piece.
Preferably, the bottom of first sampling jar is provided with the first efferent duct for exporting the hot liquid phase sample
Line, the bottom of second sampling jar are provided with the second export pipeline for exporting the cold liquid phase sample, and top is provided with
For exporting the third export pipeline of the gas phase sample.
Preferably, the on-line period device further includes：First sampling valve, first sampling valve setting take described first
Between sample tank and second sampling jar；And second sampling valve, second sampling valve are arranged in first sampling jar and institute
It states between high-temperature high-voltage reaction device.
Preferably, sampling method is provided on the pipeline for being connected to the high-temperature high-voltage reaction device of second sampling valve
Orchid, the sampling flange is to be connected to the high-temperature high-voltage reaction device.
Preferably, the high-temperature high-voltage reaction device includes paste state bed reactor or fluidized-bed reactor.
Another aspect of the present invention also provides a kind of on-line period method, including：It is mixed by what is exported in high-temperature high-voltage reaction device
It closes sample collection and the mixing sample is separated into hot phase sample into the first sampling jar, and in first sampling jar
Product, solid phase sample and hot liquid phase sample；The hot phase sample collection isolated in first sampling jar is taken to second
In sample tank, and the hot phase sample is separated into gas phase sample and cold liquid phase sample in second sampling jar.
Preferably, the mixing sample in first sampling jar settle and separate at the hot phase sample and slurries phase
Sample；And filter is set in first sampling jar, the slurry liquid phase sample is separated into the solid phase sample and institute
State hot liquid phase sample.
Preferably, the temperature of first sampling jar is made to be higher than the temperature of second sampling jar, it is preferable that described first
The temperature of sampling jar is not less than 130 DEG C, it is preferable that the temperature of second sampling jar is not higher than 3 DEG C.
Through the above technical solutions, the present invention provides a kind of on-line period device and method, the sampling of the device and method
Process does not influence the normal operation of high-temperature high-voltage reaction device.First sampling jar of on-line period device is able to receive directly from high temperature
High-pressure reactor output gas-liquid-solid three-phase mix sample, and will mixing sample be separated into hot phase sample, solid phase sample and
Hot liquid phase sample.Hot phase sample therein can be exported to the second sampling jar, and be separated into gas phase sample through the second sampling jar
Product and cold liquid phase sample.In this way, solid phase sample sampling and hydrothermal solution phase sample may be implemented from the first sampling jar, taken from second
Gas phase sample sampling and the sampling of cold liquid phase sample may be implemented in sample tank.That is, device and method through the invention, it can
It effectively realizes gas-liquid-solid three-phase separation sampling, significantly facilitates the analysis test of subsequent sample.Also, sampling operation process is simple,
Short the time required to sampling, sampling system closure is good, and toxic and harmful gas will not be revealed in sampling process.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of on-line period device according to the present invention；
Fig. 2 is the partial cutaway schematic of the first sampling jar according to the present invention；
Fig. 3 is the structural schematic diagram of filter septum according to the present invention.
Description of symbols
1 first sampling jar 11 pushes up 111 first flange of tank
12 bottom tank, 121 second flange
13 filter septum, 131 filter screen
16 heating member, 17 first export pipeline
2 second sampling jars
26 27 second export pipeline of cooling piece, 28 third export pipeline
3 first sampling valve, 4 second sampling valve 5 samples flange
Specific embodiment
Below in conjunction with attached drawing, detailed description of the preferred embodiments.It should be understood that this place is retouched
The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
Referring to figs. 1 to Fig. 3, the present invention provides a kind of on-line period device, to the high-temperature high-voltage reaction from normal operation
Gas-liquid-solid three-phase is extracted in device and mixes sample, and mixing sample is separated into gas phase sample, liquid phase sample and solid phase sample.Institute
It takes gas phase sample to can be directly used for gas chromatographic analysis, takes solid content in hot, cold conditions liquid phase sample<0.1w% takes solid
Phase catalyst particulate samples can be used to the analysis of catalyst through simple process.
With reference to Fig. 1, on-line period device of the invention includes the first sampling jar 1.First sampling jar 1 is for receiving from height
The mixing sample of warm high-pressure reactor output.In sampling operation, high-temperature high-voltage reaction device is in normal operating condition.With slurry
For bed fischer-tropsch reactor, the usual range of reactor parameter is pressure 0.5MPa-3MPa, 150 DEG C -270 DEG C of temperature.Due to anti-
It answers in device that there are high pressures, therefore can use the pressure difference between reactor and the first sampling jar 1, realize the gas-liquid made in reactor
Gu the promotion of three-phase mixing sample is drained into the first sampling jar 1.After the mixing sample of high temperature enters in the first sampling jar 1, only need
A few minutes are stood, the quick separating of the hot phase sample and slurry liquid phase sample in mixing sample can be realized.It is heavy to starch liquid phase sample
It drops to below hot phase sample.Then, it is further separated in the first sampling jar 1, it can be achieved that will slurry liquid phase sample point
From at solid phase sample and hot liquid phase sample.
On-line period device of the invention further includes the second sampling jar 2.Second sampling jar 2 is for receiving from the first sampling
The hot phase sample that tank 1 exports.Mix the sample hot phase sample and lower layer of quick separating at upper layer in the first sampling jar 1
After starching liquid phase sample, it can use the pressure difference between the first sampling jar 1 and the second sampling jar 2, push away the hot phase sample on upper layer
It is dynamic to be discharged into the second sampling jar 2.Hot phase sample temperature in the second sampling jar 2 reduces, low-carbon hydro carbons and water vapour condensation
It separates to form cold liquid phase sample with gas phase sample afterwards.
By above-mentioned, solid phase sample sampling and hydrothermal solution phase sample can be realized from the first sampling jar 1, from the second sampling
Tank 2 realizes gas phase sample sampling and the sampling of cold liquid phase sample.In this way, gas-liquid-solid three-phase mixing sample be split into gas phase sample,
Liquid phase sample and solid phase sample.It thereby not only can safely, effectively complete the on-line period to high-temperature high-voltage reaction device, moreover it is possible to
It realizes that different phase efficiently separates in sample, significantly facilitates the analysis test of subsequent sample.
With reference to Fig. 1.Some components (such as heavy wax) are easy to happen solidification because temperature declines in sample, although mixing sample
Temperature in entrained reactor can fight to a certain extent the generation of this solidification phenomenon, it is nonetheless possible to taking
The problem of sample is unsmooth or even blocking pipeline.According to the preferred embodiment of the present invention, the intake pipeline and first of the first sampling jar 1
The outside of sampling jar 1 is equipped with heating member 16.The heating member 16 is such as, but not limited to can be the structure type of electric heater, can also
To be the structure type of interlayer, etc. that hot gas source can be made to pass through.Selectively, the export pipeline of the first sampling jar 1 is also set
There is heating member 16.Preferably, the heating temperature of heating member 16 is 130 DEG C or more.By the way that heating member 16 is arranged, so that the first sampling
Always enough temperature are able to maintain in tank 1, so as to prevent that sample solidification occurs because sampler temperature declines, in turn
Pipeline is caused to block., can also be using the embodiment that is equal with heating member 16 in addition to above-mentioned preferred embodiment, such as it can be with
First sampling jar 1 is directly placed in the gas bath environment or liquid bath environment with 130 DEG C or more of temperature, etc., all it is
Variant embodiment of the invention.
According to the preferred embodiment of the present invention, the outside in the intake pipeline of the second sampling jar 2 and/or the second sampling jar
2 are equipped with cooling piece 26.The cooling piece 26 is such as, but not limited to can be the structure type of cooling jacket.Preferably, cooling piece
26 cooling temperature is 3 DEG C or less.The pressure difference between the first sampling jar 1 is more readily formed in second sampling jar 2 of low temperature, so that
Hot phase sample is easier to enter in the second sampling jar 2.Also, because being provided with cooling piece 26, hot phase sample is second
Temperature rapid decrease in sampling jar 2, low-carbon hydro carbons and water vapour separate after being condensed into liquid with the gas phase sample of low temperature, thus real
The separation of existing gas phase sample and cold liquid phase sample.It is worth noting that, may occur due to water freezing when temperature is lower than 0 DEG C
Caused pipeline blockage, therefore the control means such as cooling temperature and cooling time should be taken to avoid this unfavorable situation hair
It is raw., can also be using the embodiment being equal with cooling piece 26 in addition to above-mentioned preferred embodiment, such as second can be sampled
Tank 2 is directly placed in refrigerator, etc., is all variant embodiment of the invention.
It continues to refer to figure 1.On-line period device of the invention further includes the first sampling valve 3.First sampling valve 3 setting exists
Between first sampling jar 1 and the second sampling jar 2, the second sampling jar 2 is input to from the first sampling jar 1 to control hot phase sample
Speed and quantity.First sampling valve 3 can be hand-operated valve, be also possible to motor-driven valve or hydraulic valve.The control of first sampling valve 3
Parameter can be obtained from the detection instrument being arranged on the first sampling jar 1 and the second sampling jar 2.For example, in the first sampling in Fig. 1
It is provided with pressure gauge on valve 1 and the second sampling jar 2, the flow velocity of hot phase sample can be controlled by controlling the size of pressure
And flow.In addition, the circulation of the heat supply gas phase sample between the first sampling jar 1 and the second sampling jar 2 is arranged in the first sampling valve 3
On pipeline, the intake pipeline of previously described second sampling jar 2 can be in particular to from first the 3 to the second sampling jar of sampling valve 2
Entrance between pipeline.Cooling piece 26 is laid in the external of intake pipeline of the second sampling jar 2, hot phase sample can be made to exist
Fast cooling is begun to before into the second sampling jar 2, to accelerate the speed of gas-liquid separation.
As shown in fig. 1, on-line period device of the invention further includes the second sampling valve 4.Second sampling valve 4 setting exists
Between first sampling jar 1 and high-temperature high-voltage reaction device, to control hot mixing sample from reactor to the speed of the first sampling jar 1
And quantity.Second sampling valve 4 can be hand-operated valve, be also possible to motor-driven valve or hydraulic valve.The control parameter of second sampling valve 4 can
To be obtained from the detection instrument being arranged on the first sampling jar 1 and reactor.In addition, the second sampling valve 4 is arranged in high temperature and pressure
On the pipeline for gas-liquid-solid mixing sample flow between reactor and the first sampling jar 1, as previously mentioned, the first sampling jar 1
Intake pipeline is equipped with heating member 16, is included at the second sampling valve 4 and also sets heating member 16, prevents gas-liquid-solid mixing sample the
Phenomena such as frozen plug occurs at two sampling valves 4.
Referring still to Fig. 1, embodiment according to the present invention, the second sampling valve 4 is connected to high-temperature high-voltage reaction device
Sampling flange 5 is provided on pipeline, the sampling flange 5 is to be connected to high-temperature high-voltage reaction device.Flange 5 is sampled by setting,
The entrance of on-line period device can be quickly and easily connected to reactor；And reaction is connected to by the way that flange 5 will be sampled
The different location of device may be implemented to be sampled for the different parts of reactor.In addition, sampling flange is arranged in high temperature and pressure
On the pipeline for gas-liquid-solid mixing sample flow between reactor and the first sampling jar 1, previously described first sampling jar 1
Intake pipeline, can in particular to from sampling the 5 to the first sampling jar of flange 1 entrance between pipeline.In the first sampling jar 1
Intake pipeline sets heating member 16, at a temperature of can occurring during entering the first sampling jar 3 to avoid gas-liquid-solid mixing sample
Drop and blocking.
Referring to figs. 1 to Fig. 3.When carrying out on-line period to high-temperature high-voltage reaction device, since the operating condition of reactor is special and mixed
It is complicated to close sample composition, therefore in the prior art in order to guarantee that the standing sedimentation partition method pair of traditional conservative is usually taken in safety
Sample is separated.The special work of (such as micron-sized catalyst granules) small for some solid granularities, liquid medium large viscosity
Condition, tiny solid particle is difficult to realize effectively sedimentation in slurries phase, therefore is difficult to realize efficiently separating for liquid phase and solid phase.It is right
In common operating condition, efficiently separated even if can be realized using the separation method of gravitational settling, it is also desirable to make sample in separation system
Middle sufficient standing, it is too long so as to cause single sample time, it makes troubles to sampling operation.
According to the preferred embodiment of the present invention, it is provided with filter in the first sampling jar 1, liquid phase sample will be starched
It is separated into solid phase sample and hot liquid phase sample.Gas-liquid-solid mixing sample enter the first sampling jar 1 after, settle and separate at upper layer heat
The slurry liquid phase sample of gas phase sample and lower layer；The liquid phase sample in liquid phase sample is starched under pressure promotion by filter, separation
Below to filter；Solid phase sample in slurry liquid phase sample is stayed in above filter by filter obstruction, realize solid phase sample and
The separation of hot liquid phase sample.It, can be by tiny solid particle from big viscosity by the way that the filtering accuracy of filter is accurately arranged
Liquid medium in separate, so that solid phase sample and hot liquid phase sample thoroughly be separated.The setting side of filter
Formula can there are many, such as, but not limited to, can the top of the first sampling jar 1 be arranged lid structure, by filter be arranged grow up
The concave structure of neck, bottom extend to the lower part of the first sampling jar 1.Mixing sample can be in the concave shaped cavity that filter is formed
Settle and separate continues to separate at hot phase sample and slurry liquid phase sample, slurry liquid phase sample in the bottom of filter, forms solid phase sample
Product and hot liquid phase sample.After every sub-sampling, cover-opening structure can be beaten and take out filter, solid phase sample is removed from filter
Product.
Preferably, as depicted in figs. 1 and 2, the first sampling jar 1 includes top tank 11 and bottom tank 12.It pushes up tank 11 and bottom tank 12 can
The connection types such as releasably connect, including be bolted, be clamped.Filter is arranged to the structure type of filter septum 13, connection
Position between top tank 11 and bottom tank 12.In this way, top tank 11 and bottom tank 12 need to only be dismantled after every sub-sampling, so that it may
To take out filter septum 13, solid phase sample is removed from filter septum 13.The volume size for pushing up tank 11 and bottom tank 12 can root
It is determined according to parameters such as quantity, the general proportions of hot liquid phase sample for mixing sample when every sub-sampling.The filtration system being consequently formed
Structure is simple and convenient to operate.
Preferably, as depicted in figs. 1 and 2, the edge for pushing up tank 11 is provided with first flange 111, the edge setting of bottom tank 12
There is second flange 121, the edge of filter septum 13 is clamped between first flange 111 and second flange 121.Pass through setting first
Flange 111 and second flange 121 can easily realize that top tank 11 and bottom tank 12 are detachably connected.Furthermore it is also possible to make to push up
Tank 11 and bottom tank 12 become replaceable part.As long as first flange 111 and second flange 121 are arranged to wildcard structure, so that it may
The top tank 11 of any volume and bottom tank 12 are fitted together.As long as, so that it may difference is assembled into according to different sampling demands
First sampling jar 1 of form, promotes the scope of application of online sampler.Also, filter septum 13 is also easy to fix in.
Preferably, as shown in Figures 2 and 3, filter screen 131 is arranged in the central area of filter septum 13.That is, not
Entire filter septum 13 is all manufactured with filtering material, but uses filter material in the central area for mainly playing its filtering function
The biggish other materials manufacture of intensity can be used in the fringe region for mainly playing fixed function in matter manufacture.It so both can be with
The connection reliability of filter septum 13 is improved, and the manufacturing cost of filter septum 13 can be reduced.
In addition, according to the preferred embodiment of the present invention, filter screen 131 is wire mesh, and the wire mesh is by wire
It works out, it can be achieved that micron-sized secondary filter, solid phase sample is blocked in 131 surface of filter screen and forms filter cake, pure
Hot liquid phase sample is separated by filter screen 131.Also, it, can be by certain since wire mesh has biggish intensity
Buffer brake blowback is implemented to filter screen 131 or backwash is cleaned, may be reused filter screen 131.It is preferred that
Ground, the material for working out filter screen 131 can be metal powder sintered material either stainless steel material.It should be understood that
It is that also can choose other metal materials appropriate, is all the simple deformation of the preferred embodiment for the present invention.It is according to the present invention
Embodiment, the filtering accuracy of filter screen 131 are 25 microns to 45 microns.The filtering accuracy of filter screen 131 is by solid in reactor
The partial size of body particle determines, should ensure that the particle no more than 1w% passes through filter screen 131.
With reference to Fig. 1, embodiment according to the present invention, the bottom of the first sampling jar 1 is provided with for heat outputting liquid phase sample
First export pipeline 17 of product.Since the group that heavy wax etc. easily solidifies is divided into the main component of liquid phase sample, institute as shown in figure 1
It states, the first export pipeline 17 is equipped with heating member 16, to prevent the pipeline blockage of the first export pipeline 17.On first export pipeline 17
Valve is set, to control sampling velocity and flow.The bottom of embodiment according to the present invention, the second sampling jar 2 is provided with
For exporting the second export pipeline 27 of cold liquid phase sample.The ingredient that the cold liquid phase sample formed is condensed by hot phase sample is main
It is low-carbon hydro carbons and water, is not susceptible to the solidification as hot liquid phase sample, so need not be heated outside the second export pipeline 27.
Meanwhile temperature is too low leads to water freezing appearance in order to prevent, the second export pipeline 27 can not set cooling piece 26.Second
Valve is set on export pipeline 27, to control sampling velocity and flow.Embodiment according to the present invention, the second sampling jar 2
Top be provided with the third export pipeline 28 for exporting gas phase sample.Valve is set on third export pipeline 28, to control
Sampling velocity and flow processed.
To sum up, on-line period device of the invention can realize gas phase sampling by third export pipeline 28, pass through filtering
Partition 13 realizes solid phase sampling, realizes liquid phase sampling by the first export pipeline 17 and the second export pipeline 27.According to the present invention
Embodiment, above-mentioned high-temperature high-voltage reaction device includes paste state bed reactor or fluidized-bed reactor.
Another aspect of the present invention also provides a kind of on-line period method, including the mixing that will be exported in high-temperature high-voltage reaction device
Mixing sample is separated into hot phase sample, solid phase sample into the first sampling jar 1, and in the first sampling jar 1 by sample collection
Product and hot liquid phase sample；By the hot phase sample collection isolated in the first sampling jar 1 into the second sampling jar 2, and
Hot phase sample is separated into gas phase sample and cold liquid phase sample in two sampling jars 2.Preferably, mixing sample is in the first sampling jar
Settle and separate is at hot phase sample and slurry liquid phase sample in 1；Filter is set in first sampling jar 1, liquid phase sample point will be starched
From at solid phase sample and hot liquid phase sample.
As previously mentioned, the temperature of the first sampling jar can preferably be made to be higher than the temperature of the second sampling jar, make the first sampling jar
Temperature be not less than 130 DEG C, make the temperature of the second sampling jar not higher than 3 DEG C.
The following are the embodiments that on-line period method according to the present invention is sampled.
In diameter 1m F- T synthesis paste state bed reactor, reactor pressure 2.0MPa, 250 DEG C of temperature.It is in reactor
The form that gas-liquid-solid three-phase coexists, wherein gas holdup about 50%, gas phase main component are CO, CO2、H2、H2O and lower carbon number hydrocarbons, liquid phase
Group is divided into Fischer Tropsch waxes, and solid is fischer-tropsch synthetic catalyst particle, and solid concentration is 10w% in slurries phase (solid phase+liquid phase),
Solid grain size 40um-180um.It is realized and is connected using the sampling flange 5 and slurry bed system of DN20 model, the heating of heating member 16
Temperature is 130 DEG C or so.The material of filter septum 13 uses metal powder sintered material, precision 30um.Cooling piece 26 it is cold
But temperature is 3 DEG C or so.
All valves of confirmation on-line period device are in closed state, and sample tap is deep into inside reactor, passes through
Sample the fast and effective connection that flange 5 realizes on-line period device and paste state bed reactor.When sampling, the second sampling valve 4 is opened,
Gas-liquid-solid three-phase mixing sample in reactor enters the first sampling between reactor and the first sampling jar 1 under the promotion of pressure difference
In tank 1；Then, the second sampling valve 4 is closed.Since the first sampling jar 1 and its input and output pipeline are equipped with heating member 16, aggregate sample
Product are not in solidification phenomenon in sampling line and the first sampling jar 1.It is several to mix standing after sample enters in the first sampling jar 1
Minute, quick separating may be implemented in hot phase sample and slurry liquid phase sample during standing in sample.First sampling jar 1
Provided with filter septum 13, the hot liquid phase sample starched in liquid phase sample can pass through 13 center of filter septum under the promotion of pressure difference
The filter screen 131 in region enters 1 lower part of the first sampling jar, and starches the solid phase sample in liquid phase sample and then obstructed by filter screen 131
On the top of the first sampling jar 1.The first sampling valve 3 is slowly opened, the hot phase sample in the first sampling jar 1 is in the first sampling jar
1 and the second pressure difference between sampling jar 2 promotion under enter in the second sampling jar 2.It is applied outside second sampling jar 2 and intake pipeline
Equipped with cooling piece 26, hot phase sample temperature rapid decrease after entering the second sampling jar 2.Lighter hydrocarbons and water in hot phase sample
Vapour condenses to form cold liquid phase sample, realizes efficiently separating for gas-liquid two-phase.The valve opened on third export pipeline 28 can be realized
Sampling to gas phase sample, the sampling to hot liquid phase sample can be realized by opening the valve on the first export pipeline 17, open second
Valve on export pipeline 27 can realize the sampling to cold liquid phase sample.The connection between open top can 11 and bottom tank 12 is played, is taken out
Filter septum 13 is, it can be achieved that sampling to solid phase sample.
It is described the prefered embodiments of the present invention in detail above in conjunction with attached drawing, still, the present invention is not limited thereto.At this
It, can be with various simple variants of the technical solution of the present invention are made in the range of the technology design of invention.Including each particular technique
Feature is combined in any suitable manner.In order to avoid unnecessary repetition, the present invention is to various combinations of possible ways
No further explanation will be given.But it should also be regarded as the disclosure of the present invention for these simple variants and combination, belongs to the present invention
Protection scope.
Claims (14)
1. a kind of on-line period device, including：
First sampling jar (1), first sampling jar (1) receive the mixing sample exported from high-temperature high-voltage reaction device, will be described
Mixing sample is separated into hot phase sample, solid phase sample and hot liquid phase sample；And
Second sampling jar (2), second sampling jar (2) receive the hot phase sample exported from first sampling jar (1),
The hot phase sample is separated into gas phase sample and cold liquid phase sample.
2. on-line period device according to claim 1, which is characterized in that be provided in first sampling jar (1)
Filter mutually separates the solid phase sample with the hot liquid phase sample.
3. on-line period device according to claim 2, which is characterized in that first sampling jar (1) includes detachable
The top tank (11) and bottom tank (12) of ground connection, the filter are filtering of the setting between top tank (11) and bottom tank (12)
Partition (13).
4. on-line period device according to claim 3, which is characterized in that the edge of top tank (11) is provided with first
The edge of flange (111), the bottom tank (12) is provided with second flange (121), and the edge of the filter septum (13) is clamped in
Between the first flange (111) and the second flange (121).
5. on-line period device according to claim 3 or 4, which is characterized in that the center of the filter septum (13)
Domain is provided with filter screen (131)；The filter screen (131) is wire mesh, and the filtering accuracy of the filter screen (131) is 25 micro-
Rice is to 45 microns.
6. on-line period device according to claim 1, which is characterized in that the intake pipeline of first sampling jar (1),
The export pipeline of first sampling jar (1) of the outside and selectivity of first sampling jar (1) is equipped with heating member
(16)。
7. on-line period device according to claim 1, which is characterized in that the intake pipeline of second sampling jar (2)
Outside and/or second sampling jar (2) be equipped with cooling piece (26).
8. on-line period device according to claim 1, which is characterized in that the bottom of first sampling jar (1) is arranged
There is the first export pipeline (17) for exporting the hot liquid phase sample, the bottom of second sampling jar (2), which is provided with, to be used for
The second export pipeline (27) of the cold liquid phase sample is exported, top is provided with the output of the third for exporting the gas phase sample
Pipeline (28).
9. on-line period device according to claim 1, which is characterized in that the on-line period device further includes：First
Sampling valve (3), first sampling valve (3) are arranged between first sampling jar (1) and second sampling jar (2)；And
Second sampling valve (4), second sampling valve (4) are arranged between first sampling jar (1) and the high-temperature high-voltage reaction device.
10. on-line period device according to claim 9, which is characterized in that second sampling valve (4) is connected to institute
It states and is provided with sampling flange (5) on the pipeline of high-temperature high-voltage reaction device, the sampling flange (5) is to be connected to the high temperature and pressure
Reactor.
11. on-line period device according to claim 1, which is characterized in that the high-temperature high-voltage reaction device includes slurry
Bed reactor or fluidized-bed reactor.
12. a kind of on-line period method, including：
The mixing sample exported in high-temperature high-voltage reaction device is collected into the first sampling jar (1), and in first sampling
The mixing sample is separated into hot phase sample, solid phase sample and hot liquid phase sample in tank (1)；
By the hot phase sample collection isolated in first sampling jar (1) in the second sampling jar (2), and in institute
It states in the second sampling jar (2) and the hot phase sample is separated into gas phase sample and cold liquid phase sample.
13. on-line period method according to claim 12, which is characterized in that the mixing sample is in first sampling
Settle and separate is at the hot phase sample and slurry liquid phase sample in tank (1)；And
Filter is set in first sampling jar (1), the slurry liquid phase sample is separated into the solid phase sample and described
Hot liquid phase sample.
14. on-line period method according to claim 12 or 13, which is characterized in that make the temperature of first sampling jar
Higher than the temperature of second sampling jar, it is preferable that the temperature of first sampling jar is not less than 130 DEG C, it is preferable that described the
The temperature of two sampling jars is not higher than 3 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710339229.1A CN108871838A (en) | 2017-05-15 | 2017-05-15 | On-line period device and on-line period method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710339229.1A CN108871838A (en) | 2017-05-15 | 2017-05-15 | On-line period device and on-line period method |
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| Publication Number | Publication Date |
|---|---|
| CN108871838A true CN108871838A (en) | 2018-11-23 |
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