CN108489909A - A kind of the carbon deposition quantity of catalyst on-line measuring device and method of methanol-to-olefins process - Google Patents
A kind of the carbon deposition quantity of catalyst on-line measuring device and method of methanol-to-olefins process Download PDFInfo
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- CN108489909A CN108489909A CN201810143979.6A CN201810143979A CN108489909A CN 108489909 A CN108489909 A CN 108489909A CN 201810143979 A CN201810143979 A CN 201810143979A CN 108489909 A CN108489909 A CN 108489909A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
Abstract
The invention discloses a kind of carbon deposition quantity of catalyst on-line measuring device of methanol-to-olefins process and methods, and this approach includes the following steps：1) spectral signal of catalyst sample in reaction process is obtained by spectrum data gathering system, and extracts optical index data from spectral signal, and data are fed to data processing system；2) the carbon deposition quantity data of catalyst are estimated by model by optical index data.The carbon deposition quantity of catalyst in MTO reaction process can quickly be estimated using this method, can be used for process conditions tuning and the optimal control of process of MTO reaction process.
Description
Technical field
The present invention relates to the online detection instruments and method of a kind of methanol-to-olefins (MTO) process catalyst carbon deposition quantity, special
It is not the MTO processes using molecular sieve catalyst, the product of catalyst can be determined by the optical index of on-line determination catalyst
Carbon amounts.
Background technology
Methanol-to-olefins (MTO) industrial process uses SAPO-34 and ZSM-5 equimolecular sieve catalysts.The microcosmic ruler of catalyst
It is mainly made of the cage body of the microchannel of certain structure and connection microchannel on degree, in MTO reaction process, the reactants meeting such as methanol
The active intermediate (such as multiple methyl arene) that specific structure is first generated in catalyst cage or in microchannel, to form catalysis
Activated centre.The multiple methyl arene being trapped in catalyst cage body is one of the dominant species for constituting catalytic active center, more methyl
Aromatic hydrocarbons is both to generate the important medium of alkene and alkane, and form the presoma of carbon distribution.The reactants such as methanol constantly diffuse to
Activated centre step-reaction conversion, and controlled by " the selecting type " in catalyst duct and generate low-carbon alkene product.Meanwhile activated centre
Multiple methyl arene may also be reacted by cyclisation, hydrogen migration etc. with olefin hydrocarbon molecules and further generate stable condensed-nuclei aromatics class object
Matter, this kind of inactive condensed-nuclei aromatics will be blocked in catalyst cage body and duct, be inactivated so as to cause carbon distribution.
The experimental results show that MTO catalyst carbon distribution process can be divided into three phases：Quick carbon distribution induction period, uniformly
Carbon distribution phase, carbon distribution rapid deactivation phase.Induction period is shorter in MTO reactions, and reactant meeting fast reaction in fresh catalyst is formed
Activated centre shows as quick carbon distribution；It is interim in uniform carbon distribution, under the conditions of keeping reactant high conversion, low-carbon alkene (ethylene
+ propylene) selectivity can with catalyst carbon deposition quantity slowly improve and be stepped up, can be continuously decreased after reaching maximum value,
The corresponding carbon deposition quantity of catalyst of selectivity of light olefin maximum value can be referred to as " best carbon deposition quantity "；When catalyst carbon deposition is to centainly
The carbon distribution rapid deactivation phase is put into after degree, methanol conversion and selectivity of light olefin can drastically reduce, until carbon distribution is thorough
Inactivation (should build methanol and alkene transformation power research Zhejiang University, Hangzhou, 2015 on .SAPO-34 and ZSM-5 catalyst).
Carbon distribution inactivation catalyst can after high temperature is made charcoal circular regeneration.MTO catalyst carbon distribution and activity, selectivity of product, catalyst
Efficiency and service life are closely related, are the critical issues during MTO.It therefore, need to be to catalyst carbon deposition in MTO industrial reactors
Amount is strictly controlled.
General catalyst carbon deposition weight testing method is to burn carbon method, and the catalyst of carbon distribution is carried out calcination, is then used not
Same method measures CO, CO after calcination2And H2The amount of O determines the quantity, group of coke on catalyst further according to this tittle
At and the information such as hydrogen-carbon ratio.CO2Generally use injection method, electrical conductivity method, potentiometric titration, infrared ray gas analyzer method,
Gas chromatography etc. is detected.Han Zhongxiang etc. quantifies combustion product CO using gas chromatography2Amount to being quantitatively catalyzed
(chemical analysis measures the carbon deposition quantity of agent, 2010,19 (5):49-51).CO can also be used2There is very strong feature at 4260nm
The characteristic of absorption, using infrared gas analyser quantitative analysis CO2Production quantity, it is accurate to be carried out to the carbon deposition quantity of catalyst
Measure (petrochemical industry, 2008,37 (4):402-406).
Thermogravimetric (TG) method is also a kind of catalyst carbon deposition weight testing method of standard, and carbon deposition catalyst sample is placed in hot day
On flat, the thermogravimetric curve (TG curves) of sample is measured under the conditions of temperature programming, in air atmosphere, carbon distribution on catalyst can be by
Burning weight loss is walked, the carbon deposition quantity of catalyst can be estimated by weightless ratio.
The test method of above-mentioned carbon deposition quantity of catalyst is offline sampling analysis method, and analysis time, time-consuming, data lag
Seriously, it is simply possible to use in the after-action review to reactor, is not used to care diagnostic and the optimal control of industrial process.About catalysis
The online measuring technique of agent carbon deposition quantity is also rarely reported, and only has the disclosure of sound wave detecting method, patent CN101603950A at present
It is proposed with CN102192955A, using acoustical signal processing device reception reactor or internal regenerator catalyst ram wall surface
The acoustic emission signal of generation, in conjunction with the associated eigenvalue for being filtered acquisition catalyst carbon deposition signal accordingly, and to related special
Value indicative return the prediction model of determining carbon deposition quantity of catalyst.It is insensitive to carbon deposition quantity of catalyst in view of sonic detection technology,
The research for only staying in laboratory, without practical application.
Currently, the carbon deposition quantity of catalyst of industry MTO reactors is all made of offline sample detecting, time and effort consuming, data lag
Seriously, care diagnostic and the optimal control of industrial process are not used to.There is an urgent need for a kind of effective online catalyst carbon depositions quickly to examine
Survey method ensures the stable operation of device to monitor the operation conditions of MTO reaction units in time, is conducive to MTO reactors
The optimal control of process conditions tuning and process.
Invention content
In order to solve industrial MTO reactors carbon deposition quantity of catalyst problem on line detection, the present invention proposes one kind and adopts
The method for estimating carbon deposition quantity of catalyst with on-line determination catalyst spectral property, can be in MTO reaction process using this method
Carbon deposition quantity of catalyst quickly estimated, can be used for process conditions tuning and the optimal control of process of MTO reaction process.
The present invention provides the on-line measuring device and method of carbon deposition quantity of catalyst in a kind of MTO reaction process, specifically includes：
1) on-line period system.Solid catalyst particle sample is sampled.
2) spectrum data gathering system.It is mainly made of light source and spectrum sensor, obtains the spectrum letter of catalyst sample
Number, and data are fed to data processing system.
3) data processing system.Based on the prediction model for returning determining carbon deposition quantity of catalyst, by feeding the spectrum come letter
Number estimates the carbon deposition quantity data of catalyst through model.
The online test method of carbon deposition quantity of catalyst of the present invention can be applied to different fluid bed MTO reaction systems
In.MTO catalyst based on different catalytically active, used fluidized-bed reactor type slightly have difference, include riser,
The reactors such as fast fluidized bed, turbulent fluidized bed, multistage fluidized bed and mobile fluid bed.Without solid in same fluidized-bed reactor
The concentration difference of catalyst is larger.
The online test method of carbon deposition quantity of catalyst of the present invention can be applied to not high dilute of solid catalysis agent concentration
Phase fluid bed MTO reaction systems.The carbon deposition quantity of catalyst of dilute-phase fluidized bed is measured and includes：It is needed first through on-line period system
System takes out solid catalyst particle sample；Catalyst sample is collected in sample cell after separating gas phase, which uses
Heat resistant transparent silica glass material is made；Optical data acquisition is carried out to sample cell；Having acquired the catalyst sample after data can
By purging return mechanism.On the one hand special consideration should be given to will consider solid catalyst particle with catalyst on-line period system needs
Conveying and gas solid separation, on the other hand, since spectrum data gathering system cannot be contacted directly with the catalyst sample of high temperature,
Also need to consider the cooling heat preservation of sample and heat-insulated.
The online test method of carbon deposition quantity of catalyst of the present invention also directly can apply the MTO of high catalyst concentration anti-
Answer system.If there are the emulsion zones of catalyst in reaction system, can directly be urged using the insertion of heat safe optic-fiber combustion sensor
Agent emulsion zone carries out online spectrum data gathering, in this way can be to the product of the hot catalyst granules in reactor or regenerator
Carbon amounts is directly detected.This catalyst original position sampling method can omit the on-line period system of aforementioned cumbersome catalyst.
In heat safe optic-fiber combustion sensor, a part of fiber array is responsible for the light of light source importing reaction system and is radiated at close phase
Catalyst particle surface, while a part of optical fiber and reflectance spectrum is exported into spectrum data gathering system.
In the online test method of carbon deposition quantity of catalyst of the present invention, spectrum data gathering system includes mainly irradiation
Light source and optical sensor are all made of the light source and optical sensor of visible light wave range, wave-length coverage 360-780nm.
In the online test method of carbon deposition quantity of catalyst of the present invention, the carbon deposition quantity of catalyst in data processing system
Prediction model to be that the result measured based on carbon deposition quantity standard analytical process return determining.Carbon deposition quantity standard analytical process is optional
From in thermogravimetry, make charcoal-chromatography or-Infrared Analysis of making charcoal.
Compared with prior art, the technical advantage that can be obviously brought using the technology of the present invention includes：
1) present invention can carry out on-line analysis to carbon deposition quantity of catalyst in MTO reaction systems, can delicately react and urge in time
The changing rule of agent carbon deposition quantity；
2) operation conditions for monitoring MTO reaction units in time, ensures the stable operation of device；
3) there is positive effect for the optimal control of the process conditions tuning of MTO reaction units and process.
Description of the drawings
Fig. 1 is the L values of catalyst with the changing rule of carbon deposition quantity；
Fig. 2 is a values of catalyst with the changing rule of carbon deposition quantity；
Fig. 3 is the b values of catalyst with the changing rule of carbon deposition quantity；
Fig. 4 is estimated the BP neural network model structure of carbon deposition quantity by catalyst optical index；
Fig. 5 is dilute-phase fluidized bed MTO catalyst carbon deposition quantity on-line measuring device schematic diagram；
Fig. 6 is close phase MTO catalyst carbon deposition quantity on-line measuring device schematic diagram.
Specific implementation mode
In order to obtain the prediction model of carbon deposition quantity of catalyst, the phase between carbon deposition quantity of catalyst and the optical index of catalyst
Closing property is the theoretical foundation of the present invention, it is necessary to obtain the correlation of carbon deposition quantity of catalyst and catalyst optical index first.Invention
People simulates industrial reaction condition using industrial catalyst, and a large amount of MTO has been carried out in miniature fluidized-bed reactor experimental provision
Reaction experiment is investigated, and the catalyst under different residence-time conditions is collected, to obtain the catalyst of different carbon deposition quantities.One side
Face measures the carbon deposition quantity of catalyst using the method for thermogravimetric, while the optical index of catalyst is measured using colour photometer.Specific step
It is rapid as follows：
1) the miniature fluid bed experimental provisions of catalyst that MTO reactions prepare different carbon deposition quantities include feeding part, gasification
Device, fluidized-bed reactor and product analysis part.Miniature fluid bed internal diameter 19mm, long 350mm, reactor top are equipped with filter
To prevent the loss of catalyst, 0.5~5g catalyst is loaded every time.Before reaction starts, catalyst is under 500 DEG C, nitrogen purging
Activation 1 hour, is then adjusted to reaction temperature；Methanol aqueous solution enters vaporizer after high voltage and constant current pump-metered, is taken in nitrogen
Enter reactor with lower, through gas distributor and catalyst haptoreaction；It is rapid to stop methanol charging after certain reaction time,
Stop heating, switching nitrogen is purged 10 minutes, to blow away the reactant adsorbed on catalyst, then taken out with certain carbon deposition quantity
Catalyst.The carbon deposition quantity of catalyst is controlled by controlling the different reaction time.
2) carbon deposition quantity of catalyst measures and measures carbon deposition quantity of catalyst using thermogravimetric analyzer (SDT Q600), specific to divide
Analysis condition is：Air mass flow 100mlmin-1 rises to 800 DEG C from room temperature with the heating rate of 10 DEG C of min-1.According to thermogravimetric
Curve determines the carbon deposition quantity of catalyst.
3) carbon deposition quantity of catalyst measures the light that measures catalyst using HunterLab UltraScan VIS color difference meters
Learn index, wave-length coverage 360-780nm.Mapping is shown in Fig. 1 respectively for L values, a values and b values and the catalyst carbon deposition distribution analyzed
~3.Three parameter L values, a values and the b values of catalyst chromatic value are analyzed with the correlation of carbon deposition quantity of catalyst respectively.
L values, a values and b values are the colour space coordinate for representing the chromatic value of object color, that is, the color, any color
There is unique coordinate value.Wherein L values represent bright gray scale (black and white), and the bigger value the brighter；A values represent red green, and positive value indicates inclined
Red, negative value indicates partially green；B values represent champac color, and positive value indicates partially yellow, and negative value indicates partially blue.
As shown in Figure 1, L values and carbon deposition quantity can set up the very high linear relationship of the degree of correlation, and (R is flat for linearly dependent coefficient
Side) up to 0.938, which can be represented simply as：
Carbon deposition quantity (wt%)=21.3-0.244*L (1)
As shown in Figure 2, a values of catalyst and the degree of correlation of carbon deposition quantity be not high, this also illustrates, in visible reflectance spectrum
In, the red green feature difference of catalyst is little.
From the figure 3, it may be seen that there are significant non-linear dependencies for the b values and the carbon deposition quantity of catalyst of catalyst, using Gauss
Function Fitting relationship between the two, related coefficient (R squares) is up to 0.86, and matched curve is referring to Fig. 3.
The present invention carries out the relationship of tri- coloration value parameters of L, a and b and carbon deposition quantity using BP neural network model non-
Linear regression, used BP neural network model structure is as shown in figure 4, main structure parameters are shown in Table 1.By to BP nets
The structure of network and training have obtained average relative error and have been less than 5% catalyst prediction model, and correlation model parameters are shown in Table 2.
1. neural network main structure parameters of table
Table 1.BP neural network model parameters
It, can according to the model that the correlation between optical index L, a, the b value and carbon deposition quantity of catalyst of catalyst is established
To estimate carbon deposition quantity of catalyst using the optical index of catalyst, and for the on-line checking of carbon deposition quantity of catalyst.
Embodiment 1
Currently, common fluidized-bed reactor has quick stream in large-scale methanol-to-olefins (MTO) industrial installation
Change bed and turbulent fluid bed reactor, apparent gas phase velocity is high in reactor operating process, and catalyst concn is dilute.It can be to reactor
Interior catalyst carries out on-line period analysis, and specific on-line period analysis system schematic device is urged as shown in Figure 4, including online
Agent sampling system, optical data acquisition system and data processing system.Online catalyst sampling system is by sampling guiding valve, gas-solid
Separator, sample cell and circulating fan composition.On-line period analysis includes following steps：
1) ensure that circulating fan is opened and blow down valve is closed, be first turned on sampling guiding valve, circulating valve, carry and urge in fluid bed
The Dual-Phrase Distribution of Gas olid of agent sucks sampling system by sample tap.
2) Dual-Phrase Distribution of Gas olid gas phase after gas-solid separating device returns to fluid bed, the solid catalysis of recycling through circulating fan
Agent is collected in sample cell.
3) sampling guiding valve and circulating valve are closed immediately after completing sample collection, carry out optical data acquisition and are completed at data
Reason obtains carbon deposition quantity of catalyst data.
4) sampling guiding valve and blow down valve are opened immediately after having acquired the optical data of catalyst, by the catalyst in sample cell
Purging returns to fluidized-bed reactor, and source purge gas is low pressure water vapor.
Because the catalyst sample amount needed for analysis is small (5~10g), above-mentioned steps can be at 3 seconds after mixing automatic control system
Left and right is completed, and can be neglected compared with the catalyst residence times of hour rank in reactor, can be considered that high-fidelity samples, institute
The carbon distribution data measured are also online real time data.
Sample cell is made of heat safe optical quartz glass in system, the temperature that can be born due to light source and optical sensor
Degree condition is limited, need to catalyst sample pond using temperature control appropriate and Insulation (<180℃).What sample cell used blows
Scavenging source is low pressure water vapor, on the one hand can meet temperature control demand, simultaneously as being rich in water vapour during MTO, will not be polluted
Reaction system.
It is sampled, and used using above-mentioned catalyst on-line period analytical equipment in a certain MTO industrial reactors
The chromaticity index of line colorimetric analysis instrument analysis of catalyst is respectively：L=57.54, a=0.22, b=15.34, using above-mentioned mould
The carbon deposition quantity of the catalyst of type estimation is 7.5%.Control sampling use the thermogravimetric analysis of standard obtain the carbon deposition quantity of catalyst for
7.38%, error 1.6%.Illustrate the reliability of the online test method.
Embodiment 2
To in large-scale methanol-to-olefins (MTO) industrial installation, there is also the emulsion zones of catalyst, such as fluid bed
The close phase heat transfer zone of reactor wall surface heat exchanger is removed the close phase buffering area of catalyst charcoal regeneration device by fluid bed MTO reactors
Deng.
It can directly use heat safe optic-fiber combustion sensor to be inserted into catalyst emulsion zone in the emulsion zone of catalyst to carry out
Linear light modal data acquires, and specific device schematic diagram is as shown in Figure 5.Compared with Example 1, this catalyst original position sampling method can
Cumbersome catalyst on-line period system is omitted, is more convenient simple.
In heat safe optic-fiber combustion sensor, a part of fiber array is responsible for the light of light source importing reaction system and be shone
It penetrates in dense-phase catalyst particle surface, while a part of optical fiber and reflectance spectrum is exported into spectrum data gathering system.With reality
It applies example 1 to compare, the carbon distribution data measured by the device are exactly online real time data.
Claims (7)
1. a kind of carbon deposition quantity of catalyst online test method of methanol-to-olefins process, which is characterized in that include the following steps：
1) spectral signal of catalyst sample in reaction process is obtained by spectrum data gathering system, and is carried from spectral signal
Optical index data are taken, and data are fed to data processing system；
2) the carbon deposition quantity data of catalyst are estimated by model by optical index data.
2. the carbon deposition quantity of catalyst online test method of methanol-to-olefins process according to claim 1, which is characterized in that
The spectral signal is the reflectance spectrum that is obtained by optical sensor after light source irradiates catalyst sample；
The optical index data include three parameter L values, a values and the b values of reflected light chromatic value.
3. the carbon deposition quantity of catalyst online test method of methanol-to-olefins process according to claim 1, which is characterized in that
The light source optical sensor is all made of the light source and sensor of visible spectrum, wave-length coverage 360-780nm.
4. the carbon deposition quantity of catalyst online test method of methanol-to-olefins process according to claim 1, which is characterized in that
Catalyst sample to be measured is located at fluid bed dilute-phase zone；
Solid catalyst particle sample is taken out by on-line period system, catalyst collection measures in suprasil sample cell
Spectral signal in sample cell；
After optical data acquisition finishes, catalyst sample is by purging return mechanism.
5. the carbon deposition quantity of catalyst online test method of methanol-to-olefins process according to claim 1, which is characterized in that
Catalyst sample to be measured is located at fluid bed emulsion zone；
It is imported light by heat safe fibre optical sensor and is radiated at catalyst particle surface, and reflectance spectrum exported to visible
Optical sensor.
6. a kind of on-line measuring device for realizing Claims 1 to 5 any one of them method, which is characterized in that including：
Spectrum data gathering system, the spectral signal for obtaining the sample, and optical index number is extracted from spectral signal
According to optical index data are then fed to data processing system；
Data processing system, for receive by spectrum data gathering System feeder Lai light optical index data, while being based on back
The prediction model for returning determining carbon deposition quantity of catalyst calculates the carbon deposition quantity of catalyst.
7. on-line measuring device according to claim 6, which is characterized in that further include for solid catalyst particle sample
The on-line period system that product are sampled.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110514600A (en) * | 2019-09-05 | 2019-11-29 | 内蒙古中煤蒙大新能源化工有限公司 | A kind of measuring method of MTO catalyst carbon content |
| CN114076803A (en) * | 2020-08-21 | 2022-02-22 | 国家能源投资集团有限责任公司 | Method for detecting carbon deposition composition of catalyst |
| CN114076803B (en) * | 2020-08-21 | 2024-04-30 | 国家能源投资集团有限责任公司 | Method for detecting carbon deposit composition of catalyst |
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