CN109738572A - A kind of catalyst performance evaluation device and evaluation method - Google Patents
A kind of catalyst performance evaluation device and evaluation method Download PDFInfo
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- CN109738572A CN109738572A CN201811587211.4A CN201811587211A CN109738572A CN 109738572 A CN109738572 A CN 109738572A CN 201811587211 A CN201811587211 A CN 201811587211A CN 109738572 A CN109738572 A CN 109738572A
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Abstract
The invention discloses a kind of catalyst performance evaluation device and evaluation methods, including reaction system, have at least one reactor, and reactor is equipped with sample tap；Raw material mixing system contains at least three interfaces including at least one and has the container of a constant volume, and wherein at least one interface is used to individually connect with the raw material of one of mixed raw material simple substance component；Raw material feed system is connect by flow control system with raw material mixing system；On-line analysis system is connected by the sample tap of sampling line and reaction system；Whistle control system is mutually communicated with human-computer interaction interface and flow control system, to make the ratio of each component in mixed raw material up to setting value according to the ratio automatic control flow control system of each component in the raw material set in man-machine interface.The present invention can make catalyst sample accurately and under stable raw material carry out performance evaluation in component proportion, while can also flexibly and accurately feed change form, and finally obtain more stable performance evaluation number.
Description
Technical field
The present invention relates to catalyst performance evaluation technical fields, fill more specifically to a kind of catalyst performance evaluation
It sets and evaluation method.
Background technique
In chemical production process, overwhelming majority chemical reaction is realized by the help of catalyst.Being of catalyst
One of the core technology of most critical in work production process, the performance of catalyst decide that can a kind of production process be realized, and
Its economy.
A kind of research and development of catalyst, generally will be by small-scale experiment, pilot plant test and industry amplification application test.Its
In, the small-scale experiment stage needs performance comparison by a large amount of screening and repeatedly.These mostly tests are by simulated production work
The catalyst test apparatus of skill is completed.For at present, evaluated using performance of the evaluating apparatus to catalyst sample
It is the most reliable means that properties of sample is known in catalyst R&D process.
The evaluation data of catalyst will have convincingness, it is of great importance that, the state of arts of catalyst test apparatus
Need stable as far as possible, the composition of especially raw material is required to reach more stable state.However since catalyst is commented
The size of valence device has the difference of the order of magnitude compared with commercial plant, and raw material flow is smaller, so wanting to the precision of raw material control equipment
Ask higher, while again because its internal space is smaller, lower for the redundant ability of technological fluctuation, the above a variety of causes be will cause
The raw material composition of catalyst test apparatus is not very stable, and then affects the accuracy and repeatability of evaluating catalyst data, often
Puzzlement often is caused to the experiment work of catalyst.
In the prior art, some attempts to realize the configuration of mixed raw material, but the reality of mixed raw material by mass flowmenter
Border component situation is not known.Some is reacted by first configuring gaseous mixture, then with prepared gas source, some components are in container
In have change of gradient or time change, do not ensure that the stabilization of raw material components, while can not timely change component yet
Ratio.
Summary of the invention
The technical problem to be solved in the present invention is that the raw material composition and component proportion of existing evaluating apparatus are unstable,
Therefore a kind of catalyst performance evaluation device and evaluation method are provided, can provide accurate component proportion mixed raw material and
Flexibly accurately feed change forms.
The technical solution adopted by the present invention to solve the technical problems is: a kind of catalyst performance evaluation device, including
Reaction system, including at least one reactor, the reactor are equipped with sample tap；
Raw material mixing system contains at least three interfaces including at least one and has the container of a constant volume, wherein extremely
A few interface is used to individually connect with the raw material of one of mixed raw material simple substance component；
Raw material feed system is connect by the flow control system on multiple pipelines with raw material mixing system；
On-line analysis system is connected by the sample tap of sampling line and reaction system；
Whistle control system is mutually communicated with human-computer interaction interface and flow control system, according to human-computer interaction interface
The ratio automatic control flow control system of each component, reaches the ratio of each component in mixed raw material in the raw material of setting
Setting value in human-computer interaction interface.
Preferably, the reactor includes reaction tube, heater, insulating layer and temperature element, the sample tap is set
In on reaction tube, the insulating layer is located in reaction tube, and the heater is used to heat for reaction tube, and the temperature element is used for
Measure the temperature of reaction tube.
Preferably, the raw material feed system is composed of more than one material container, or by more than all the way
Supply lines be composed or the two combination.
Preferably, the reaction system further includes having pressure detecting element, the pressure detecting element is pressure gauge, pressure
One of power transmitter and pressure sensor are a variety of.
Preferably, tube inner diameter/catalyst sample equivalent diameter > 3.
Preferably, at least one described temperature element can measure the temperature of reaction pipe outer wall.
Preferably, at least one described temperature element can measure the temperature of reaction tube.
Preferably, at least one described temperature element is capable of the temperature on HEATER FOR MEASURING surface.
Preferably, having heat tracing on the sampling line of the sample tap connection, heat tracing is coated on by thermal insulation material and is taken
On sample pipeline.
Preferably, the material after the reacted system response can be by flowing out after pressure stabilizing device, the pressure stabilizing is set
It is standby to use electrohydraulic pressure control regulating valve, the rear end Tandem mass flowmeter of the electrohydraulic pressure control regulating valve.
A kind of catalyst performance evaluation method includes the following steps: using catalyst performance evaluation equipment as described above
(1) catalyst sample is measured, is put into the reactor in reaction system；
(2) according to requirement of experiment, in the composition ratio of human-computer interaction interface setting raw material；
(3) on-line analysis system is opened, analysis instrument reaches normal assay state；
(4) from raw material feed system to raw material mixing system base feed；
(5) the raw material composition ratio that whistle control system is set according to human-computer interaction interface, according to on-line analysis system
Value of feedback is analyzed, flow control system is adjusted, up to the analysis value of feedback of the raw material components ratio after raw material mixing system mixes
Reach requirement of experiment；
(6) catalysis reaction occurs for the catalyst in the reacted system of mixed raw material, and the material after reaction passes through online
Analysis system is analyzed, and communication of the result through whistle control system is analyzed, and is exported to human-computer interaction interface, according to human-computer interaction
The evaluation performance data of catalyst sample can be obtained in the analysis data shown on interface.
Preferably, when the simple substance component raw material individually being connect with raw material mixing system in the step (4), it is at least one
Be after final mixing in raw material volumetric concentration be more than 3% each simple substance component in the minimum component of content, concentration and finally mix
The ratio of the highest simple substance component of volumetric concentration content is 1: 5~1: 20 in raw material after conjunction.
Implement a kind of catalyst performance evaluation device of the invention and evaluation method, has the advantages that the present invention
Catalyst sample can be made accurately and under stable raw material to carry out performance evaluation in component proportion, while can also flexibly and accurately be changed
Become raw material composition, finally obtains more stable performance evaluation data.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples, in attached drawing:
Fig. 1 is a kind of frame structure schematic diagram of catalyst performance evaluation device of the invention；
Fig. 2 is a kind of frame structure schematic diagram of catalyst performance evaluation device of the embodiment of the present invention one.
Specific embodiment
For a clearer understanding of the technical characteristics, objects and effects of the present invention, now control attached drawing is described in detail
A specific embodiment of the invention.
It should be noted that in the description of the present invention, term " on ", "front", "rear", "left", "right", " is erected at "lower"
Directly ", the orientation or positional relationship of the instructions such as "horizontal", "top", "bottom", "inner", "outside" is orientation based on the figure or position
Relationship is set, is merely for convenience of description of the present invention and simplification of the description, is not that device or the element of indication or suggestion meaning are necessary
It with specific orientation, is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.In addition, term
" first ", " second " etc. are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
As shown in Figure 1, in a kind of embodiment of catalyst performance evaluation device of the invention, including reaction system 1, original
Expect hybrid system 2, raw material feed system 3, flow control system 4, on-line analysis system 5, whistle control system 6 and human-computer interaction
Interface 7, reaction system 1 include at least one reactor, and reactor is equipped with sample tap, and raw material mixing system 2 includes at least one
Containing at least three interfaces and with the container of a constant volume, wherein at least one interface is used for single with one of mixed raw material
The raw material of matter component individually connects；Raw material feed system 3 passes through the flow control system 4 and raw material mixing system on multiple pipelines
2 connections；On-line analysis system 5 is connect by sampling line with the sample tap of reaction system 1；Whistle control system 6 and man-machine friendship
Mutual interface 7 and flow control system 4 mutually communicate, with the ratio of each component in the raw material that set according to human-computer interaction interface 7 oneself
Dynamic control flow control system 4, makes the ratio of each component in mixed raw material reach the setting value in human-computer interaction interface 7.
In catalyst performance evaluation device in the present invention, reaction system 1 is by more than one reactor group at reactor can
To be any one or more in currently available technology in already present structure, and at least one reactor be by reaction tube,
The compositions such as heater, insulating layer and temperature element, as tube inner diameter/catalyst sample equivalent diameter > 3, have more preferable
Evaluation effect.Catalyst sample equivalent diameter refers to: the sieve screening catalyst sample of two layers of different aperture size is selected,
The big sieve of middle relative porosity factor is upper, and under, pore shape is square the small sieve of relative porosity factor, when the upper sieve of selection
Net enables the catalyst sample of quality accounting 80% to pass through, and lower screen makes the catalyst sample fallen by upper screen
The catalyst sample of quality accounting 80% can not pass through in product, then two layers of sieve respectively hole average side length value be added divided by
2 be catalyst sample equivalent diameter.
Temperature element in reaction system 1 needs to measure the surface of the outer wall of reaction tube, the inner wall of reaction tube and heater
Temperature, therefore, at least one temperature element can measure the temperature of the outer wall of reaction tube, at least one temperature element energy
The temperature of the inner wall of reaction tube is enough measured, and at least one temperature element is capable of the temperature on the surface of HEATER FOR MEASURING.
In order to preferably control pressure, reaction system 1 further includes having pressure detecting element, and pressure detecting element can be with
It is one of pressure gauge, pressure transmitter and pressure sensor or a variety of.
Material after reacted system 1 is reacted can be by flowing out after pressure stabilizing device.Pressure stabilizing device uses electrohydraulic pressure control tune
Valve is saved, pressure feedback is provided by the pressure detecting element in reaction system 1.Flow can also be connected in the rear end of pressure stabilizing device
Meter.
Raw material mixing system 2 is connected with reaction system 1, what the container with a constant volume in raw material mixing system 2 referred to
It is that, using the flow direction of raw material after mixing as linear measure longimetry direction, the internal cavities volume of container is greater than to connect the pipeline of container rule
Lattice are foundation, the volume after equal length calculating.For example, the pipeline internal diameter of connection container is 6mm, container is with raw material after mixing
It is 150mm that flow direction, which is orientation measurement length, then the volume that the volume of the container is greater than 150mm, internal diameter is 6mm pipeline is about
4.24ml.In addition, at least one is former after final mixing when the simple substance component raw material individually connecting with raw material mixing system 2
In material volumetric concentration be more than 3% each simple substance component in the minimum group timesharing of content, then all compositions in raw material after final mixing
Ratio can faster and more accurately reach stable state, and if make a change the operation of composition ratio, after final mixing
The ratio of all compositions can also faster and more accurately reach stable state again in raw material.Preferably, above-mentioned one kind is final
After mixing in raw material volumetric concentration be more than 3% each simple substance component in the minimum component of content, concentration with finally mix after original
The ratio of the highest simple substance component of volumetric concentration content is 1: 5~1: 20 in material, and effect is best.
Raw material feed system 3 passes through flow control system 4 and 2 phase of raw material mixing system by the multichannel pipeline above all the way
Even, to provide raw material for device.Raw material feed system 3 can be the combination of more than one material container, be also possible to all the way
Above supply lines combination, is also possible to the two combination.Sample pre-treatments equipment, which has, reduces free water content
Component.
Flow control system 4 is by with the integral type flow controller or flowmeter of flow measurement function and the combination of regulating valve
It constitutes.Mass flow controller can be used, for example, thermal mass flow controller can be used.
Raw material mixing system 2 is connected with reaction system 2, and mixed raw material is by reaction system 1, in the effect of catalyst
Under, it chemically reacts.For material after reaction by flowing out after pressure stabilizing device pressure stabilizing, pressure stabilizing refers to pressure before stablizing, that is, reacts
The pressure of system 1.Pressure stabilizing device can use manual counterbalance valve or electrohydraulic pressure control regulating valve.For example, electrohydraulic pressure control can be used
Regulating valve, pressure feedback are provided by the pressure measuring element of reaction system 1.For example, it is also possible in electrohydraulic pressure control regulating valve
Rear end Tandem mass flowmeter, by changes in flow rate trend, operator can preferably judge raw material flow in reaction process
Stability.
The outlet rear end of each reactor has between raw material mixing system 2 and reaction system 1 and in reaction system 1
There is sample tap, the medium drawn from sample tap is connected by sampling line with on-line analysis system 5.On-line analysis system 5 can
The composition ratio of medium in each sampling line is analyzed, and these analysis results are transferred to whistle control system 6.As preferred
Technical solution, there is pressure stabilizing device, pressure or rear pressure before can stablizing on sampling line.
Data are more accurately analyzed in order to obtain, any component condensation in the medium in sampling line should be prevented, because
This, sampling line can have heat tracing, and heat tracing mode is steam or electric heating.Heat tracing and sampling line can be wrapped up by thermal insulation material
Together.Heat tracing temperature should in a certain range, and temperature upper limit should be no more than the heat of any component in medium in sampling line
Decomposition temperature, lowest temperature should be not less than the condensation temperature of any component in medium in pipeline.
On-line analysis system 5 is made of one or more analysis instrument and sample pre-treatments equipment, and analysis instrument can be with
It is gas-chromatography, liquid chromatogram, infrared spectrum analyser, magnetic oxygen analyser, the mass spectrograph with Multi-channel switching valve or more single-passes
Road mass spectrograph etc..Sample pre-treatments equipment is at least made of components such as filter, pressure maintaining valve, flowmeters.For containing free water
Sampling line in medium, sample pre-treatments equipment should also have the component for reducing free water content, such as moisture separator.
Whistle control system 6 is used for and human-computer interaction interface 7 and the mutually communication respectively of flow control system 4, operator
The ratio of each component in raw material is set using human-computer interaction interface 7, whistle control system 6 can be set according to human-computer interaction interface 7
The ratio of each component in fixed raw material, the ratio of each component in flow automatic regulation control system 4 make each in mixed raw material
The ratio of component reaches the setting value in human-computer interaction interface 7.
Whistle control system 6 can be all tools such as distributed control module, programmable logic controller (PLC), one-chip computer module
Standby acquisition analog quantity, digital quantity signal, data processing and output analog quantity, the control module of digital quantity signal.
Human-computer interaction interface 7 is a kind of software module, can be realized and shows the various types of signal that the transmission of whistle control system 6 comes
Show to operator, the information that operator inputs can also be exported to whistle control system 6.
The invention also discloses a kind of evaluation methods of catalyst performance evaluation device, include the following steps:
(1) catalyst sample is measured, is put into the reactor in reaction system 1；
(2) according to requirement of experiment, the composition ratio of raw material is set in human-computer interaction interface 7；
(3) on-line analysis system 5 is opened, analysis instrument reaches normal assay state；
(4) from raw material feed system 3 to 2 base feed of raw material mixing system；
(5) the raw material composition ratio that whistle control system 6 is set according to human-computer interaction interface 7, according to on-line analysis system 5
Analysis value of feedback, adjust flow control system 4, until through raw material mixing system 2 mixing after raw material components ratio analysis it is anti-
Feedback value reaches requirement of experiment；
(6) catalysis reaction occurs for the catalyst in the reacted system 1 of mixed raw material, and the material after reaction passes through online
Analysis system 5 is analyzed, and communication of the result through whistle control system 6 is analyzed, and is exported to human-computer interaction interface 7, according to man-machine
The evaluation performance data of catalyst sample can be obtained in the analysis data shown on interactive interface 7.
The present invention will be further described below by way of examples.But following examples are only simple example of the invention
Son, does not represent or limits the scope of the present invention, and interest field of the invention is subject to claims.
Embodiment one
One, catalyst test apparatus
As shown in Fig. 2, catalyst test apparatus includes reaction system 1, raw material mixing system 2, raw material feed system 3, stream
Amount control system 4, on-line analysis system 5, whistle control system 6 and human-computer interaction interface 7, reaction system 1 is by a reactor
Composition, reactor are made of a reaction tube, a set of electric heater, insulating layer, three thermocouples and a pressure sensor, instead
Should pipe outer diameter be 6.35mm, internal diameter 3.86mm.Three thermocouples can measure the outer of reaction tube as temperature element respectively
The temperature of wall, the inner wall of reaction tube and heater surfaces.The outlet of reactor be equipped with electric pressure-regulating valve, by on reactor
Pressure sensor constitute control loop, the internal pressure of reactor can be stablized.
Raw material mixing system 2 is connected with reaction system 1 by 1/4 inch of outer diameter of pipeline, and raw material mixing system 2 is by one
There are six the gas mixers of interface to form for band, and the outer diameter of the gas mixer is 12.7mm, internal diameter 10.2mm, six interfaces
In five interfaces through flow control system 4, totally 5 gas bombs are connect with Q1~Q5 in raw material feed system 3 respectively, reaction
When by Q5~Q1 order mixed raw material, wherein store in Q1 be after final mixing in raw material volumetric concentration be more than 3% it is each
The minimum component raw material of content in simple substance component.Flow control system 4 is using 5 thermal mass flow controller branch controls 5
The flow of road gas.
In the present embodiment, reactor between raw material mixing system 2 and reaction system 1 and in reaction system 1 goes out
Mouth rear end all has sample tap, and the medium drawn from sample tap is connected by sampling line with on-line analysis system.Every road sampling
Pipeline all has electric tracing, and highest heat tracing temperature is no more than 120 DEG C.Sampling line first has to by sample pre-treatments case.The case
It is interior to contain filter, pressure maintaining valve, spinner flowmeter and dehumidifier.
Sampling line is connected after the processing of sample pre-treatments case with a mass spectrograph with Multi-channel switching valve, different
Sampling line is separately connected analysis channel different on magnetic fan formula mass spectrum.The mass spectrograph is controlled through signal through transmission line and signal
System 6 and human-computer interaction interface 7 mutually communicate, and whistle control system 6 is distributed using the ECS-700 for controlling production in Zhejiang
Control system, using the ratio of each component in the raw material of the setting of human-computer interaction interface 7, whistle control system 6 can be according to man-machine friendship
The ratio of each component in the raw material that mutual interface 7 is set, the ratio of each component in flow automatic regulation control system 4, after making mixing
Raw material in the ratio of each component reach the setting value in human-computer interaction interface 7.Human-computer interaction interface 7 is using by ECS-
700 included configuration softwares.
Two, evaluating catalyst method
Evaluation test can be carried out to multiple catalysts using the equipment in the embodiment above, here with ethylene ring
For oxidative ethane catalyst, evaluating catalyst method is as follows:
(1) equivalent diameter is the catalyst sample 2g of 1.0mm after weighing crushing and screening in the balance, is seated in reaction system 1
In reactor in reaction tube in, measure practical filling height, going out admission space according to PIPE DIAMETER CALCULATION is 1.8ml；
(2) in the ratio of the setting raw material composition of human-computer interaction interface 7: ethylene 32%, oxygen 7.5%, carbon dioxide 1%,
1,2- dichloroethanes 1.2ppm (mol), nitrogen 59.5%；
(3) air speed for being 5000h-1 according to reaction condition in human-computer interaction interface 7 sets the total flow of mixed raw material gas
For 0.25NL/min, reaction pressure 1.8MPa, reaction temperature is 220 DEG C；
(4) mass spectrograph opened in on-line analysis system 5 is preheated, until mass spectrograph self-test reaches normal assay shape
State；
(5) Q1~Q5 in raw material feed system 3 respectively corresponds oxygen, carbon dioxide, by the 1 of accounting 50ppm (mol),
2- dichloroethanes and gaseous mixture, ethylene and nitrogen remaining as nitrogen；
The raw material composition ratio that whistle control system 6 is set according to human-computer interaction interface 7, according to on-line analysis system 5
Value of feedback is analyzed, flow control system 4 is adjusted, until the analysis of raw material components ratio is practical after the mixing of raw material mixing system 2
Value reaches requirement of experiment.
Catalyst generation catalysis reaction in the mixed reacted system 1 of raw material, generation ethylene oxide and carbon dioxide,
The by-products such as water, the material after reaction are analyzed by on-line analysis system 5, analyze communication of the result through whistle control system 6, defeated
Out to human-computer interaction interface 7, research staff obtains catalyst sample according to the analysis data shown on human-computer interaction interface 7
Evaluate performance data.
Evaluating the most important data of ethylene epoxy ethane catalyst performance is ethylene oxide space-time yield and ring
Oxidative ethane selectivity, calculation method are as follows:
Note: EO finger ring oxidative ethane, Δ EO mol%=export EO mol%- entrance EO mol%,
Wherein the calculation method of air speed is as follows:
Embodiment two
The difference is that, do not have probe tube between raw material mixing system 2 and reaction system 1 with embodiment one
Line, only offline sample tap, device is unable to after on-line analysis mixes each component ratio in raw material, and then cannot be fed back according to analysis
Value automatically adjusts the feed rate of each component raw material, and the situation of mixed raw material can only be judged by the result of off-line analysis,
Then component ratio is adjusted by changing flow.
Embodiment three
The difference is that, the outer diameter of reaction tube is 4mm, internal diameter 2.54mm with embodiment one.
Example IV~embodiment seven
The difference is that, the mixed order of each component raw material is different with embodiment one, see the table below:
Implementation result comparison
Matched with feeding intake in 24 hours raw material components ratio overall average deviation ratio to measure embodiment with comparative example raw material components
The Stability and veracity of ratio, to feed intake, the standard deviation of ethylene oxide space-time yield and ethylene oxide selectivity in 24 hours is measured
The stability of embodiment and comparative example performance evaluation data, sampling period are half an hour.
Wherein the calculation method of raw material components ratio overall average deviation ratio is as follows:
The Contrast on effect of one~embodiment of embodiment seven is as follows:
Embodiment eight
One, catalyst test apparatus
A kind of catalyst test apparatus includes reaction system 1, raw material mixing system 2, on-line analysis system 5, signal control
System 6, human-computer interaction interface 7, raw material feed system 3 and flow control system 4, reaction system 1 by three reactor groups at,
Each reactor is by a reaction tube, a set of electric heater, insulating layer, a thermocouple and a pressure sensor group
At the outer diameter of reaction tube is 12.7mm, internal diameter 10.21mm.Wherein thermocouple can measure the temperature of the outer wall of reaction tube.Instead
It answers device outlet to have manual pressure regulating valve, reactor pressure can be stablized.
Raw material mixing system 2 is connected with reaction system 1 by the pipeline that outer diameter is 1/2 inch, and raw material mixing system 2 is by one
The gas mixer of four interfaces of a band forms, and the outer diameter of gas mixer is 25.4mm, internal diameter 21mm.In four interfaces
Through flow control system 4, totally two gas bombs and Q3 pipeline are connect three interfaces with Q1, Q2 in raw material feed system 3 respectively,
By the order mixed raw material of Q3~Q1 when reaction, what is wherein stored in Q1 is that volumetric concentration is more than 3% in raw material after finally mixing
Each simple substance component in the minimum component raw material of content.Flow control system 4 uses three thermal mass flow controller branches
Control the flow of three road gases.
The outlet rear end of each reactor between raw material mixing system 2 and reaction system 1 and in reaction system 1
With sample tap, the medium drawn from sample tap is connected by sampling line with on-line analysis system 5.Every road sampling line all bands
There is electric tracing, highest heat tracing temperature is no more than 110 DEG C.Sampling line first has to by sample pre-treatments case.Contained in the case
Filter, pressure maintaining valve, spinner flowmeter and dehumidifier.
Sampling line is connected after the processing of sample pre-treatments case with an on-line chromatograph and a magnetic oxygen analyser, can be online
Obtain the component analysis value in each sampling channel.Assay value is through transmission line and whistle control system 6 and 7 phase of human-computer interaction interface
Mutually communication, whistle control system 6 using Siemens Company S7-200 programmable logic controller (PLC) (English abbreviation PLC),
The ratio of each component in raw material is set using human-computer interaction interface 7, whistle control system 6 can be set according to human-computer interaction interface 7
The ratio of each component in fixed raw material, the ratio of each component in flow automatic regulation control system 4 make each in mixed raw material
The ratio of component reaches the setting value in human-computer interaction interface 7.Human-computer interaction interface 7 is using wincc software.
Two, evaluating catalyst method
Evaluation evaluation test can be carried out to multiple catalysts using the equipment in the embodiment above, we are here with methane
For selective oxidation making formaldehyde catalyst, it is as follows that specific embodiment is described in detail:
(1) equivalent diameter is the catalyst sample 5g of 2.2mm after weighing crushing and screening in the balance, is seated in reaction system 1
In reactor in reaction tube in, measure practical filling height, going out admission space according to PIPE DIAMETER CALCULATION is 3ml；
(2) ratio of the raw material composition set in human-computer interaction interface 7: methane 72%, oxygen 7.2%, nitrogen
20.8%；
(3) in human-computer interaction interface 7 according to reaction condition 12000h-1Air speed, set the total flow of mixed raw material gas as
0.6NL/min, reaction pressure 5.0MPa, the wherein calculation method of air speed are as follows:
(4) analysis instrument opened in on-line analysis system 5 is preheated, until instrument self checking reaches normal assay shape
State；
(5) Q1~Q3 respectively corresponds oxygen, nitrogen and methane in raw material feed system 3；
(6) the raw material composition ratio that whistle control system 6 is set according to human-computer interaction interface 7, according to on-line analysis system 5
Analysis value of feedback, flow control system 4 is adjusted, until the analysis of raw material components ratio is real after the mixing of raw material mixing system 2
Actual value reaches requirement of experiment；
(7) catalysis reaction occurs for the catalyst in the reacted system 1 of mixed raw material, generates purpose product formaldehyde and one
The by-products such as carbonoxide, carbon dioxide, water, the material after reaction are analyzed by on-line analysis system 5, analyze result through signal control
The communication of system 6 processed, output to human-computer interaction interface 7, research staff according to the analysis data shown on human-computer interaction interface 7,
Obtain the evaluation performance data of catalyst sample.
The evaluation most important data of methane selectively oxidizing making formaldehyde catalyst performance are methane conversion and formaldehyde choosing
Selecting property, calculation method are as follows:
Note: ΔmolThe outlet %=mol%- entrancemol%
Embodiment nine
The difference is that, do not have probe tube between raw material mixing system 2 and reaction system 1 with embodiment eight
Line, only offline sample tap, device is unable to after on-line analysis mixes each component ratio in raw material, and then cannot be fed back according to analysis
Value automatically adjusts the feed rate of each component raw material.Operator can only judge mixed raw material by the result of off-line analysis
Situation, then adjust component ratio by changing flow.
Embodiment ten
With embodiment eight the difference is that: the outer diameter of reaction tube be 8mm, internal diameter 6mm.
Embodiment 11~13
The difference is that, the mixed order of each component raw material is different, and concrete order see the table below with embodiment eight:
Implementation result comparison
We measure embodiment and comparative example raw material group to feed intake in 24 hours raw material components ratio overall average deviation ratio
The Stability and veracity of distribution ratio is measured with the standard deviation of methane conversion and formaldehyde selectivity in 24 hours that feeds intake and is implemented
The stability of example and comparative example performance evaluation data.Sampling period is half an hour.
Wherein the calculation method of raw material components ratio overall average deviation ratio is as follows:
The Contrast on effect of eight~embodiment of embodiment 13 is as follows:
The embodiment of the present invention is described with above attached drawing, but the invention is not limited to above-mentioned specific
Embodiment, the above mentioned embodiment is only schematical, rather than restrictive, those skilled in the art
Under the inspiration of the present invention, without breaking away from the scope protected by the purposes and claims of the present invention, it can also make very much
Form, all of these belong to the protection of the present invention.
Claims (10)
1. a kind of catalyst performance evaluation device, which is characterized in that including
Reaction system, including at least one reactor, the reactor are equipped with sample tap；
Raw material mixing system contains at least three interfaces including at least one and has the container of a constant volume, and wherein at least one
A interface is used to individually connect with the raw material of one of mixed raw material simple substance component；
Raw material feed system is connect by the flow control system on multiple pipelines with raw material mixing system；
On-line analysis system is connected by the sample tap of sampling line and reaction system；
Whistle control system is mutually communicated with human-computer interaction interface and flow control system, to be set according to human-computer interaction interface
Raw material in each component ratio automatic control flow control system, so that the ratio of each component in mixed raw material is reached man-machine
Setting value in interactive interface.
2. a kind of catalyst performance evaluation device according to claim 1, which is characterized in that the reactor includes reaction
Pipe, heater, insulating layer and temperature element, the sample tap are set on reaction tube, and the insulating layer is located in reaction tube, institute
Heater is stated for heating for reaction tube, the temperature element is for measuring the temperature of reaction tube.
3. a kind of catalyst performance evaluation device according to claim 1, which is characterized in that the raw material feed system by
More than one material container is composed, or is composed of the supply lines above all the way or the two
Combination.
4. a kind of catalyst performance evaluation device according to claim 1, which is characterized in that the reaction system further includes
There is pressure detecting element, the pressure detecting element is one of pressure gauge, pressure transmitter and pressure sensor or more
Kind.
5. a kind of catalyst performance evaluation device according to claim 4, which is characterized in that
Tube inner diameter/catalyst sample equivalent diameter > 3.
6. a kind of catalyst performance evaluation device according to claim 2, which is characterized in that at least one described thermometric
Element can measure the temperature of reaction pipe outer wall；Or at least one described temperature element can measure the temperature of reaction tube
Degree；Or at least one described temperature element is capable of the temperature on HEATER FOR MEASURING surface.
7. a kind of catalyst performance evaluation device according to claim 1, which is characterized in that the sample tap connection takes
There is heat tracing, heat tracing is coated on sampling line by thermal insulation material on sample pipeline.
8. a kind of catalyst performance evaluation device according to claim 1, which is characterized in that the reacted system response
Material afterwards can be by flowing out after pressure stabilizing device, and the pressure stabilizing device uses electrohydraulic pressure control regulating valve, the electrohydraulic pressure control tune
Save the rear end Tandem mass flowmeter of valve.
9. a kind of catalyst performance evaluation method, sets using catalyst performance evaluation as described in any one of claim 1 to 9
It is standby, which comprises the steps of:
(1) catalyst sample is measured, is put into the reactor in reaction system；
(2) according to requirement of experiment, in the composition ratio of human-computer interaction interface setting raw material；
(3) on-line analysis system is opened, analysis instrument reaches normal assay state；
(4) from raw material feed system to raw material mixing system base feed；
(5) the raw material composition ratio that whistle control system is set according to human-computer interaction interface, according to the analysis of on-line analysis system
Value of feedback adjusts flow control system, until the analysis value of feedback of raw material components ratio reaches after raw material mixing system mixes
Requirement of experiment；
(6) catalysis reaction occurs for the catalyst in the reacted system of mixed raw material, and the material after reaction passes through on-line analysis
System is analyzed, and communication of the result through whistle control system is analyzed, and is exported to human-computer interaction interface, according to human-computer interaction interface
The evaluation performance data of catalyst sample can be obtained in the analysis data of upper display.
10. a kind of catalyst performance evaluation method according to claim 9, which is characterized in that in the step (4) when with
The simple substance component raw material that raw material mixing system individually connects, at least one are that volumetric concentration is more than 3% in raw material after finally mixing
Each simple substance component in the minimum component of content, concentration with finally mix after the highest simple substance group of volumetric concentration content in raw material
The ratio divided is 1: 5~1: 20.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110873777A (en) * | 2019-12-17 | 2020-03-10 | 兰州金润宏成石油化工科技有限公司 | A pilot test device for evaluating low carbon hydrocarbon oxidation catalyst performance |
| CN110940767A (en) * | 2019-11-11 | 2020-03-31 | 中国科学院金属研究所 | Device and method for researching same-position microstructure evolution of heterogeneous catalyst in gas-phase catalytic system |
| CN111089936A (en) * | 2019-12-25 | 2020-05-01 | 北京化工大学 | High-throughput catalyst performance analysis device and method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5911953A (en) * | 1996-06-14 | 1999-06-15 | Nippon Soken, Inc. | Apparatus for detecting and analyzing adsorbates |
| EP0971225A2 (en) * | 1998-07-09 | 2000-01-12 | HTE GmbH, The high throughput experimentation company | Device for detecting a product in the exhaust flow of a catalyst material of a plurality of catalyst materials |
| CN105116096A (en) * | 2015-08-13 | 2015-12-02 | 中国石油化工股份有限公司 | Hydrodeoxygenation catalyst evaluation device |
| CN205506776U (en) * | 2016-01-26 | 2016-08-24 | 华纳创新（北京）科技有限公司 | Evaluation device of SCR denitration catalyst |
| CN106596832A (en) * | 2016-06-02 | 2017-04-26 | 华纳创新（北京）科技有限公司 | SCR denitration catalyst evaluation device |
| CN207440030U (en) * | 2017-09-21 | 2018-06-01 | 中国石油天然气股份有限公司 | Denitration catalyst's contrast evaluation device |
-
2018
- 2018-12-25 CN CN201811587211.4A patent/CN109738572A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5911953A (en) * | 1996-06-14 | 1999-06-15 | Nippon Soken, Inc. | Apparatus for detecting and analyzing adsorbates |
| EP0971225A2 (en) * | 1998-07-09 | 2000-01-12 | HTE GmbH, The high throughput experimentation company | Device for detecting a product in the exhaust flow of a catalyst material of a plurality of catalyst materials |
| CN105116096A (en) * | 2015-08-13 | 2015-12-02 | 中国石油化工股份有限公司 | Hydrodeoxygenation catalyst evaluation device |
| CN205506776U (en) * | 2016-01-26 | 2016-08-24 | 华纳创新（北京）科技有限公司 | Evaluation device of SCR denitration catalyst |
| CN106596832A (en) * | 2016-06-02 | 2017-04-26 | 华纳创新（北京）科技有限公司 | SCR denitration catalyst evaluation device |
| CN207440030U (en) * | 2017-09-21 | 2018-06-01 | 中国石油天然气股份有限公司 | Denitration catalyst's contrast evaluation device |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110940767A (en) * | 2019-11-11 | 2020-03-31 | 中国科学院金属研究所 | Device and method for researching same-position microstructure evolution of heterogeneous catalyst in gas-phase catalytic system |
| CN110873777A (en) * | 2019-12-17 | 2020-03-10 | 兰州金润宏成石油化工科技有限公司 | A pilot test device for evaluating low carbon hydrocarbon oxidation catalyst performance |
| CN111089936A (en) * | 2019-12-25 | 2020-05-01 | 北京化工大学 | High-throughput catalyst performance analysis device and method |
| CN111089936B (en) * | 2019-12-25 | 2021-03-26 | 北京化工大学 | High-throughput catalyst performance analysis device and method |
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