CN107843667A - Methanol-to-olefins product two-dimensional gas chromatography on-line measuring device and method - Google Patents
Methanol-to-olefins product two-dimensional gas chromatography on-line measuring device and method Download PDFInfo
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- CN107843667A CN107843667A CN201711261994.2A CN201711261994A CN107843667A CN 107843667 A CN107843667 A CN 107843667A CN 201711261994 A CN201711261994 A CN 201711261994A CN 107843667 A CN107843667 A CN 107843667A
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- chromatographic column
- switching mechanism
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
Abstract
The present invention relates to a kind of online two-dimensional gas chromatography on-line measuring device of methanol-to-olefins product and method.A kind of methanol-to-olefins product two-dimensional gas chromatography on-line measuring device, including first pressure stable module, multichannel port valve, the first chromatographic column and the gas circuit switching mechanism being sequentially connected by pipeline, multichannel port valve are also associated with quantitative loop；The gas circuit switching mechanism is also connected with organic oxygen carrier detector, and the first pipeline and the second pipeline are connected to after gas circuit switching mechanism, detector is equipped with first pipeline and the second pipeline；First pipeline is provided with the first detector, and the second pipeline is provided with the second detector, the first pipeline be located at the first detector before pipeline on be additionally provided with the second chromatographic column；Wherein, the first chromatographic column is Lowox capillary columns, and the second chromatographic column is PLOT Q or PLOT Al2O3Chromatographic column.Present invention, avoiding oxygen-bearing organic matter to Al in chromatographic column2O3The destruction of filler.
Description
Technical field
The present invention relates to gas composition analysis equipment, more particularly to a kind of methanol-to-olefins product two-dimensional gas chromatography is online
Detection means and method.
Background technology
With methanol-to-olefins（MTO）The successful commercialization of technology, exploitation and the application of its product detection technology turn into MTO
Further business promotion and the key of technical optimization.It is therefore necessary to develop a kind of MTO products simple in construction, highly effective to exist
Line detecting system.From the point of view of the relevant information of domestic and international research report, MTO product detections use more chromatograms or more valves mostly
Group controls cutting techniques to realize, and can cause the structure of a whole set of analysis system using more chromatogram or valve and control relatively multiple
It is miscellaneous, increase the unstability of system long-term operation.
Xing Aihua exists《The quantitative analysis method of methanol to olefins reaction product is studied》It is middle to use single six-way valve and double ten-way valves
Combination coordinate double TCD detectors and double packed columns to carry out quantitative study to MTO reaction products, the set system is due to using TCD
Detector, the sensitivity detected relative to fid detector to hydrocarbons is relatively low, and to the isomer of C4 alkene therein
Can not efficiently separate it is quantitative, so Xing Aihua et al. later developments are a set of to have three ten-way valves, double FID and single TCD institutes group
Into product full constituent analysis system,《The quantitative analysis method of methanol to olefins reaction product full constituent is studied》In, Xing Aihua
Describe the set system effectively can carry out quantitative analysis to full constituent in methanol-to-olefins product.Pueraria lobota happiness it is intelligent et al.《Gas phase
Chromatography analysis methanol-to-olefins product gas full constituent》Using three six-way valves, two ten-way valves, three chromatograms are respectively provided with two
The huge analysis system of individual TCD detectors and a fid detector carries out full constituent analysis to methanol-to-olefins product.More than
These have more valve group switchings, use the analysis detection means of multi-color spectrum and multi-detector make it that analysis system is excessively complicated, hold
It is also easy to produce potential faults.Especially in the handoff procedure of valve, the pressure oscillation of carrier gas system can be caused, carrier gas pressure in chromatographic system
The stabilization of power influences significantly, to influence whether chromatogram testing result on detection process.And have in these valve control systems largely not
Rust steel pipe and joint, its high heat capacity having are unfavorable in chromatogram accurately following the trail of and stablizing chromatogram temperature, and this may be to coal
The product analysis of alkene processed produces some interference.Worked for a long time under such complex pipeline in addition and be likely to result in pipeline connection
The leakage at place, it is also possible to cause the broadening of chromatographic peak.What is more important, due to containing H2O, MeOH, DME in MTO product
Deng oxygenatedchemicals, and hydrocarbons are analyzed often with the Al contained in chromatographic column2O3Filler easily adsorbed by these oxygen carriers and
Inactivation, long-term use can damage chromatographic column.So for MTO product analysis, in order to extend the service life of chromatographic column and raising
The accuracy of analysis, it is necessary to entered back into after oxygen carrier is cut containing Al2O3Chromatographic column in analyzed, it is still, different
Operation condition of chromatogram result in the difference of oxygen carrier retention time in product to be measured, this has resulted in carrying out oxygen carrier
The difficulty of cutting, in general, in order to determine the peak sequence and appearance time of oxygen carrier under certain condition, it is necessary to
Product appearance result is investigated in carry out system and comprehensive experiment, determines clipping time according to result, this is undoubtedly caused
The complexity of experiment, reduces analysis efficiency.
The content of the invention
In order to solve the problems, such as above-mentioned MTO product detections, the present invention is intended to provide a kind of methanol-to-olefins product two-dimensional gas
Phase chromatogram on-line measuring device and method.
Technical program of the present invention lies in：
A kind of methanol-to-olefins product two-dimensional gas chromatography on-line measuring device, including the first pressure being sequentially connected by pipeline
Stable module, multichannel port valve, the first chromatographic column and gas circuit switching mechanism, multichannel port valve are also associated with quantitative loop；The gas circuit
Switching mechanism is also connected with organic oxygen carrier detector, and the first pipeline and the second pipe are connected to after gas circuit switching mechanism
Road, detector is equipped with first pipeline and the second pipeline；First pipeline is provided with the first detector, is set on the second pipeline
Have the second detector, the first pipeline be located at the first detector before pipeline on be additionally provided with the second chromatographic column；Wherein, the first chromatogram
Post is Lowox capillary columns, and the second chromatographic column is PLOT Q or PLOT Al2O3Chromatographic column.
The first described column's length 10m, internal diameter are 0.3 ~ 0.53mm, the second column's length 25-50m, internal diameter
0.25~0.32mm。
Described first pressure stable module is electron pressure control module EPC.
Second pressure stable module is additionally provided with, second pressure stable module is directly connected to gas circuit switching mechanism, the second pressure
Power stable module is startup control module PCM.
Pipeline between described multichannel port valve and the first chromatographic column is provided with hand sampling mouth.
Described the first detector and the second detector is flame ionization ditector.
Pipeline between described gas circuit switching mechanism and the second detector is provided with current limiter.
A kind of online two-dimensional gas chromatography analysis method of methanol-to-olefins product, is produced using methanol-to-olefins as described above
Thing two-dimensional gas chromatography on-line measuring device is analyzed methanol-to-olefins product, and its component of methanol-to-olefins product includes C1
~C6 hydrocarbon gas, dimethyl ether and methanol；Comprise the following steps：
The carrier gas provided by first pressure stable module, is flowed into multi-ported valve, and carrier gas flows directly into after multichannel port valve
Follow-up pipeline, quantitative loop is passed through in multi-ported valve, directly emptied；When switching multi-ported valve conducting direction, carrier gas is by quantitative loop
The sample of middle fixed amount is pushed in follow-up pipeline, and sample inlet is directly emptied by multi-ported valve；
By the switching of multi-ported valve, the sample of fixed amount is sent to the first chromatographic column by carrier gas, in the first chromatographic column first
A point analysis of variance is carried out to the oxygenatedchemicals methanol and dimethyl ether of sample；Gas is entered from the determinand of the first chromatographic column outflow
Road switching mechanism, organic oxygen-containing substance detector is provided with this gas circuit switching mechanism, when organic oxygen-containing substance detector detects
When organic oxygen carrier is free of in determinand, then the determinand is switched into the first pipeline by gas circuit switching mechanism；When organic
Oxygen carrier detector detects when containing organic oxygen carrier in determinand, then switches the determinand by gas circuit switching mechanism
To the second pipeline；The current limiter that determinand entered on the second pipeline, enter after current limiter in the second detector and examined
Survey.
The technical effects of the invention are that：
The present invention by first pressure stable module and second pressure stable module in the case of keeping nebulizer gas pressure stable,
The time of product segmentation switching is determined by the oxygen carrier detector in gas circuit switching mechanism, oxygen-containing so as to avoid
Organic matter is to Al in chromatographic column2O3The destruction of filler.
Brief description of the drawings
Fig. 1 is principle schematic diagram of the present invention.
Fig. 2 is that carrier gas is directly entered the structural representation in the case of analysis system without quantitative loop in six-way valve of the present invention
Figure.
After Fig. 3 is six path Vavle switchings of the invention, determinand in quantitative loop is sent in the case of analysis system by carrier gas
Structural representation.
Reference：P1, first pressure stable module, P2, second pressure stable module, V1, multi-ported valve, i, sample introduction
Mouthful, C1, the first chromatographic column, C2, the second chromatographic column, b, gas circuit switching mechanism, r, current limiter, d1, the first detector, d2, second
Detector.
Embodiment
As Figure 1-3, a kind of methanol-to-olefins product two-dimensional gas chromatography on-line measuring device, including by pipeline according to
The first pressure stable module P1 of secondary connection, multichannel port valve, the first chromatographic column C1 and gas circuit switching mechanism, multichannel port valve also connect
It is connected to quantitative loop；The gas circuit switching mechanism is also connected with organic oxygen carrier detector, is connected to after gas circuit switching mechanism
First pipeline and the second pipeline, detector is equipped with first pipeline and the second pipeline；First pipeline is provided with first
Detector d1, the second pipeline are provided with the second detector d2, the first pipeline be located at the first detector d1 before pipeline on also set
There is the second chromatographic column C2；Wherein, the first chromatographic column C1 is Lowox capillary columns, and the second chromatographic column C2 is PLOT Q or PLOT Al2O3
Chromatographic column.
Wherein, the first described chromatographic column C1 column length 10m, internal diameter are 0.3m ~ 0.53mm, the second chromatographic column C2 column lengths 25-
50m, 0.25 ~ 0.32mm of internal diameter.Described first pressure stable module P1 is electron pressure control module EPC.It is additionally provided with second
Pressure stability module P2, second pressure stable module P2 are directly connected to gas circuit switching mechanism, and second pressure stable module P2 is
Start control module PCM.Pipeline between described multichannel port valve and the first chromatographic column C1 is provided with hand sampling mouth i.Institute
The the first detector d1 and the second detector d2 stated is flame ionization ditector.Described gas circuit switching mechanism and
Pipeline between two detector d2 is provided with current limiter r.Above-mentioned carrier gas used is high pure nitrogen.
A kind of online two-dimensional gas chromatography analysis method of methanol-to-olefins product, is produced using methanol-to-olefins as described above
Thing two-dimensional gas chromatography on-line measuring device is analyzed methanol-to-olefins product, and its component of methanol-to-olefins product includes C1
~C6 hydrocarbon gas, dimethyl ether and methanol；Step is as follows：
The carrier gas provided by first pressure stable module P1, is flowed into multi-ported valve 3, carrier gas is directly flowed after multichannel port valve
Enter follow-up pipeline, quantitative loop is passed through in multi-ported valve 3, directly empty；When switching 3 conducting direction of multi-ported valve, carrier gas will be fixed
The sample of fixed amount is pushed in follow-up pipeline in amount ring, and sample inlet is directly emptied by multi-ported valve 3；
The carrier gas provided by electron pressure control module EPC, is flowed into six-way valve, and six-way valve is in shown in Fig. 1 during state,
Carrier gas is entered in six-way valve, is flowed directly into follow-up pipe-line system.And sample is entered in six-way valve, by quantitative loop, so
Directly empty afterwards.When six-way valve is switched to state shown in Fig. 3, the sample of fixed amount in quantitative loop is pushed to follow-up pipe by carrier gas
Lu Zhong, and sample inlet is directly emptied by six-way valve.
By the switching of multi-ported valve 3, the sample of fixed amount is sent to the first chromatographic column C1 by carrier gas, in the first chromatographic column
A point analysis of variance is carried out to the oxygenatedchemicals methanol and dimethyl ether of sample first in C1；From the to be measured of the first chromatographic column C1 outflows
Thing enters gas circuit switching mechanism, and organic oxygen-containing substance detector is provided with this gas circuit switching mechanism, when organic oxygen-containing material is examined
Survey device to detect when being free of organic oxygen carrier in determinand, then the determinand is switched into the first pipe by gas circuit switching mechanism
Road；When organic oxygen-containing substance detector, which detects, contains organic oxygen carrier in determinand, then the determinand is cut by gas circuit
Converting mechanism switches to the second pipeline；The current limiter r that determinand entered on the second pipeline, the second inspection is entered after current limiter r
Survey in device d2 and detected.
Embodiment 1
Using high pure nitrogen as carrier gas, through pressure-reducing valve by source of the gas mesohigh gas decompression to 0.5 ~ 0.6MPa or so, high pure nitrogen
It is divided into two-way, the first via is flowed into six-way valve through first pressure stable module P1, and sample gas flows into six-way valve, by quantitative
Directly emptied after ring.After six-way valve switches, carrier gas pushes the sample in verge ring into subsequent analysis pipeline, and sample inlet is then
Directly emptied by six-way valve.Original state is switched back into after sample in quantitative loop fully flows into follow-up pipeline, then by six-way valve,
This is so as to also just complete once online sample introduction process.It is repeated several times and carries out above-mentioned six-way valve handoff procedure, it is possible to achieve is continuous
Multiple online sample introduction.
It is Lowox capillary columns that sample is sent into the first chromatographic column C1, the first chromatographic column C1 by carrier gas by pipeline, column length 10m,
Internal diameter is 0.53mm.Sample is separated at this, entered from the product of the first chromatographic column C1 outflows in gas circuit switching mechanism.It is logical
Organic oxygen-containing substance detector is crossed, the pipeline flowed into sample switches over selection., can be with by second pressure stable module P2
Adjust caused pressure oscillation problem in gas circuit handoff procedure.
If not having oxygen-bearing organic matter in determinand, C1~C6 hydrocarbon components initially enter to be separated in chromatographic column 2,
Chromatographic column 2 is from PLOT Q or PLOT AL2O3Chromatographic column, column length 25-50 rice, 0.25 ~ 0.32 millimeter of internal diameter.When C1~C6 hydro carbons
Component flows completely through gas circuit switching mechanism, and the methanol and dimethyl ether in product to be measured are detected by oxygen-bearing organic matter detector,
Then gas circuit is switched to the second pipeline so that follow-up other components including methanol and dimethyl ether enter current limiter r, pass through
Enter after current limiter r in the second detector d2 and detected.
Typical chromatograph box heating and Vavle switching process are：First chromatographic column C1 and the second chromatographic column C2 initial temperatures
50 DEG C are arranged to, retains 5 minutes at 50 DEG C, 160 DEG C, then the liter with 10 DEG C/min is then increased to 4 DEG C/min speed
Warm speed is increased to 190 DEG C, is kept for 9.5 minutes at 190 DEG C.
Six-way valve switches in 0.01min, and 1min switches again.Gas circuit switching mechanism switches in 0.8min, in 3.3min again
Secondary switching.
The conversion ratio of methanol can be calculated with below equation.
Wherein X is methanol conversion（%）, CCH3OH is that methanol feeds molar flow（mol/min）, F is carrier gas N2 body
Product flow (dm3/ min), XCH3OHFor the correction factor of methanol, VlFor quantitative loop volume, ACH3OHFor the peak area of methanol.Due to
Carrier N2Volume flow F to be far longer than product and the volume flow V of unreacted methanoll, so the unit interval, methanol was in product
In total amount with the amount and F V of the methanol contained in quantitative looplProduct represent.
The molar selectivity of product with below equation to be calculated：
。
Part that the present embodiment does not describe in detail and the well-known components and often for belonging to the industry with structure and English name
With structure or conventional means, do not describe one by one here.
Claims (8)
- A kind of 1. online two-dimensional gas chromatography on-line measuring device of methanol-to-olefins product, it is characterised in that：Including passing through pipeline The first pressure stable module being sequentially connected（P1）, multichannel port valve, the first chromatographic column（C1）And gas circuit switching mechanism（b）, it is more Road port valve is also associated with quantitative loop；The gas circuit switching mechanism（b）It is also connected with organic oxygen carrier detector, gas circuit switching mechanism （b）After be connected to the first pipeline and the second pipeline, be equipped with detector on first pipeline and the second pipeline；First Pipeline is provided with the first detector（d1）, the second pipeline is provided with the second detector（d2）, the first pipeline is located at the first detector （d1）The second chromatographic column is additionally provided with pipeline before（C2）；Wherein, the first chromatographic column（C1）For Lowox capillary columns, the second color Compose post（C2）For PLOT Q or PLOT Al2O3Chromatographic column.
- 2. the online two-dimensional gas chromatography on-line measuring device of methanol-to-olefins product according to claim 1, its feature exist In：The first described chromatographic column（C1）Column length 10m, internal diameter are 0.3 ~ 0.53mm, the second chromatographic column（C2）Column length 25-50m, internal diameter 0.25~0.32mm。
- 3. the online two-dimensional gas chromatography on-line measuring device of methanol-to-olefins product according to claim 2, its feature exist In：Described first pressure stable module（P1）For electron pressure control module EPC.
- 4. the online two-dimensional gas chromatography on-line measuring device of methanol-to-olefins product according to claim 3, its feature exist In：It is additionally provided with second pressure stable module（P2）, second pressure stable module（P2）With gas circuit switching mechanism（b）It is directly connected to, Second pressure stable module（P2）To start control module PCM.
- 5. the online two-dimensional gas chromatography on-line measuring device of methanol-to-olefins product according to claim 4, its feature exist In：Described multichannel port valve and the first chromatographic column（C1）Between pipeline be provided with hand sampling mouth（i）.
- 6. the online two-dimensional gas chromatography on-line measuring device of methanol-to-olefins product according to claim 5, its feature exist In：The first described detector（d1）And second detector（d2）It is flame ionization ditector.
- 7. methanol-to-olefins product two-dimensional gas chromatography on-line measuring device according to claim 6, it is characterised in that：Institute The gas circuit switching mechanism stated（b）With the second detector（d2）Between pipeline be provided with current limiter（r）.
- A kind of 8. methanol-to-olefins product two-dimensional gas chromatography online test method, it is characterised in that：Use as above claim 7 The online two-dimensional gas chromatography on-line measuring device of described methanol-to-olefins product is analyzed methanol-to-olefins product, methanol Its component of olefin product processed includes C1~C6 hydrocarbon gas, dimethyl ether and methanol；Comprise the following steps：Pass through first pressure stable module（P1）The carrier gas of offer, is flowed into multi-ported valve（3）Interior, carrier gas is straight after multichannel port valve Connect and flow into follow-up pipeline, in multi-ported valve（3）It is middle to pass through quantitative loop, directly empty；Switch multi-ported valve（3）During conducting direction, The sample of fixed amount in quantitative loop is pushed in follow-up pipeline by carrier gas, and sample inlet directly passes through multi-ported valve（3）Emptying；Pass through multi-ported valve（3）Switching, the sample of fixed amount is sent to the first chromatographic column by carrier gas（C1）, in the first chromatographic column （C1）In a point analysis of variance is carried out to the oxygenatedchemicals methanol and dimethyl ether of sample first；From the first chromatographic column（C1）Outflow Determinand enters gas circuit switching mechanism（b）, this gas circuit switching mechanism（b）In be provided with organic oxygen-containing substance detector, when organic Oxygen carrier detector detects when organic oxygen carrier is free of in determinand, then the determinand is passed through into gas circuit switching mechanism （b）Switch to the first pipeline；When organic oxygen-containing substance detector, which detects, contains organic oxygen carrier in determinand, then this is treated Survey thing and pass through gas circuit switching mechanism（b）Switch to the second pipeline；The current limiter that determinand entered on the second pipeline（r）, pass through Current limiter（r）Enter the second detector afterwards（d2）In detected.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711261994.2A CN107843667A (en) | 2017-12-04 | 2017-12-04 | Methanol-to-olefins product two-dimensional gas chromatography on-line measuring device and method |
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