CN208366926U - Realize the device of chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization - Google Patents
Realize the device of chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization Download PDFInfo
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- CN208366926U CN208366926U CN201820435474.2U CN201820435474U CN208366926U CN 208366926 U CN208366926 U CN 208366926U CN 201820435474 U CN201820435474 U CN 201820435474U CN 208366926 U CN208366926 U CN 208366926U
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Abstract
The utility model discloses a kind of devices that can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization, including gas distribution system, pulse air gas handling system, temperature programming resistance furnace, electrochemical test system and TCD detector；Wherein gas distribution system allows the present apparatus that different functions can be achieved by changing the state of triple valve and switch valve, thus quantitatively characterizing while realizing chemical adsorption amount and chemisorption electric signal by four tunnel gas compositions.Device provided by the utility model only characterizes chemical absorption behavior better than traditional chemical adsorption instrument by adsorbance variation；The important information in chemisorption can also be captured by surface change in electric caused by aerochemistry adsorption process.
Description
Technical field
The utility model relates to a kind of new equipments for studying chemisorption, in particular for catalyst and its chemistry of carrier
The detection device of absorption.
Background technique
Heterogeneous catalysis process is to convert reaction product for reactant molecule by the circulation of primitive step.Catalytic cycle is extremely
Few includes five diffusion, chemisorption, surface reaction, desorption and reversed diffusion steps.Wherein, diffusion and Reaction-diffusion terms speed compared with
Fastly, surface reaction does not have selectivity；It can be seen that chemisorption is link mostly important in heterogeneous catalysis process.Moreover,
Absorption of the reactant molecule on catalyst surface decides the property for the degree and catalytic process that reactant molecule is activated
Matter, such as activity and selectivity.Therefore, absorption of the research reactant molecule or probe molecule on catalyst surface, for explaining
The mechanism that the principle of property, catalytic action that bright reactant molecule interacts with catalyst surface and catalysis are reacted has ten
Divide important meaning.
Chemisorption is a kind of interfacial phenomenon, for many years, characterization of the people using various modern spectroscopy technique and with routine
Means combine, from the energy of the surface texture of molecular level investigation chemisorbed layer, ADSORPTION STATE and analysis and surface action
Relationship obtains result of study extensively and profoundly, forms this important sphere of learning of Surface Science, and chemisorption also just becomes
Important component part.
In complex phase catalysis, majority belongs to surface of solids catalytic gas phase reaction, this adsorbs closely coupled with the surface of solids.?
In this kind of reaction, at least a kind of reactant is adsorbed by chemistry of solid surfaces, and the absorption is the committed step of catalysis, gas
Molecule may cause ionization, deformation etc. when chemistry of solid surfaces adsorbs, and can greatly improve their reactivity.Therefore,
Chemisorption is highly important to studying and illustrating catalytic mechanism.
Chemisorption is related with surface of solids structure, many of research of surface texture chemistry absorption characterization method, main
It to include various spectral techniques, surface profile measurement technology etc..In addition to this, laboratory facilities mainly use chemical adsorption instrument to realize
The temperature programming analytical technology (TPAT) of chemisorption.Temperature-programmed technique mainly includes temperature programmed desorption (TPD), program liter
Temperature reduction (TPR), temperature programmed oxidation (TPO), temperature programmed surface reaction (TPSR).It is urged by temperature-programmed technique in research
Desorption behavior of the molecule in heating and during various reflex actions on agent surface, can with or following important information:
Type, density and the Energy distribution at adsorption center；The combination energy and reference state of binding molecule and adsorption site；Catalyst is living
Type, density and the Energy distribution at property center；The dynamic behavior and reaction mechanism of reaction molecular；Active component and carrier, work
Interaction between property component；Various catalytic effects, catalyst inactivation and regeneration etc..
However, traditional chemical adsorption instrument is by characterizing chemical suction to the absorption variable quantity of gas during chemisorption
Attached behavior.And have one important to be characterized in during chemisorption: adsorption molecule and surface of solids atom (or molecule) are sent out
Transfer, the exchange or shared of raw electronics, form the absorption of sorption chemical key.Since there are the uneven field of force, surfaces for the surface of solids
On atom often there are also remaining bonding power, just occur between surface atom when on gas molecule collision to the surface of solids
Exchange, the transfer or shared of electronics, form the suction-operated of sorption chemical key.Therefore, can be made by gas sensing electric signal
For a kind of new method for studying chemisorption.Therefore it provides a kind of measure surface of solids adsorbance during chemisorption simultaneously
Variation with the electric signal of gas sensing is necessary to capture the device of chemisorption information.
Utility model content
In order to solve the deficiencies in the prior art, the utility model provide it is a kind of for characterizing the new equipment of chemisorption,
It can detecte the variation of gas absorption surface of solids adsorbance and electric signal caused in particular solid surface process, thus
Chemical absorption behavior can be inferred and characterized by the variation of adsorbance and absorption electric signal simultaneously.
The utility model provide it is a kind of can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization
Device, including gas distribution system, pulse air gas handling system, temperature programming resistance furnace, electrochemical test system and the inspection of TCD gas
Survey device；
The gas distribution system includes the first gas circuit, the second gas circuit, third gas circuit and the 4th gas circuit, first gas circuit
The first triple valve is connected, the other both ends of the first triple valve are separately connected pulse gas discharge pipe and first gas delivery pipe,
And mass flowmenter, check valve and switch valve are sequentially installed in first gas circuit；
Mass flowmenter, check valve and switch are sequentially installed in second gas circuit, third gas circuit and the 4th gas circuit
Valve, second gas circuit, third gas circuit and the 4th gas circuit are in parallel by first gas mixing tube, the first gas mixing tube with
The connection of TCD detector air inlet, the TCD detector exhaust outlet is connected to by pipeline with the second triple valve, described
The other both ends of second triple valve are separately connected six-way valve and second gas delivery pipe, the first gas delivery pipe and described second
Air shooter is in parallel by second gas mixing tube, the gas access of the second gas mixing tube and temperature programming resistance furnace
The gas vent of connection, described program heating resistance furnace is connect by pipeline with third triple valve, described program heating resistance furnace
It is electrically connected with electrochemical test system, the other both ends of the third triple valve are separately connected tail gas discharging pipe and third gas is defeated
Pipe is sent, the third gas delivery pipe is connected to another air inlet of TCD detector, and in the third gas delivery pipe
Portion is equipped with drying device, and another exhaust outlet of TCD detector is connected to by pipeline with the tail gas discharging pipe；Described six
Port valve is arranged on pulse gas discharge pipe；
The pulse air gas handling system and the first gas circuit, the second gas circuit, third gas circuit and the 4th air circuit connection, for the
One gas circuit, the second gas circuit, third gas circuit and the 4th gas circuit feed pulse air.
Preferably, described device further includes control computer, each flowmeter, temperature programming resistance in the gas distribution system
Furnace, electrochemical test system, TCD detector are electrically connected with control computer.
Preferably, diluent gas delivery pipe, the diluent gas delivery pipe are also connected in the second gas delivery pipe
On needle valve is installed.
Preferably, it is equipped with reaction tube and platinum electrode in described program heating resistance furnace, the reaction tube is inhaled for placing
Appendix body, the platinum electrode are used to connect the electricity outside absorption carrier and described program heating resistance furnace in the reaction tube
Test chemical system.
Preferably, the 4th air shooter, described 4th air shooter one end and institute are also connected on the six-way valve
Six-way valve connection is stated, the other end and second gas delivery pipe are connected；4th air shooter and first gas conveying
It is also connected with the 5th air shooter between pipe, mass flowmenter and unidirectional is also sequentially installed on the 5th air shooter
Valve is also equipped with switch valve in the second gas delivery pipe.
Preferably, the absorption carrier includes catalyst.
Preferably, it is carrier gas that first gas circuit, which is passed through, in second gas circuit, third gas circuit and the 4th gas circuit extremely
What rare two-way was passed through is under test gas.
Compared with prior art, the utility model has the beneficial effects that:
Gas distribution system in device provided by the utility model passes through the present apparatus by four tunnel gas compositions
Change the state of triple valve, six-way valve and switch valve different functions can be achieved, to realize that chemical adsorption amount and chemistry are inhaled
Quantitatively characterizing while attached electric signal.Device provided by the utility model is only changed by adsorbance better than traditional chemical adsorption instrument
To characterize chemical absorption behavior；Chemistry can also be captured by surface change in electric caused by aerochemistry adsorption process
Important information in absorption.In addition, device provided by the utility model is better than the common level-one distribution of traditional chemical adsorption instrument
System, second level distribution, the accurate distribution of minimum achievable 1ppm gas may be implemented in it.
Detailed description of the invention
In order to illustrate the embodiment of the utility model or the technical proposal in the existing technology more clearly, below will be to embodiment
Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is this
Some embodiments of utility model, for those of ordinary skill in the art, without creative efforts, also
Other drawings may be obtained according to these drawings without any creative labor.
Fig. 1 can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative to be provided by the embodiment of the utility model
The schematic diagram of the device of characterization.
Specific embodiment
It can be practiced in order to enable those skilled in the art to better understand the technical solutions of the present invention, below with reference to
The utility model is described in further detail for specific embodiment, but illustrated embodiment is not as the restriction to the utility model.
The device provided by the utility model that can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization,
It is specific as shown in Figure 1, include gas distribution system, pulse air gas handling system, temperature programming resistance furnace, electrochemical test system and
TCD detector；
Gas distribution system includes the first gas circuit 1, the second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4, and the first gas circuit 1 is defeated
Sending is carrier gas, and the first gas circuit 1 connects the first triple valve 101, and the other both ends of first triple valve 101 are separately connected pulse
Gas outlet pipe 102 and first gas delivery pipe 103, and be sequentially installed with mass flowmenter, check valve in the first gas circuit 1 and open
Close valve；It is sequentially installed with mass flowmenter, check valve and switch valve in second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4, the
Two gas circuits 2, third gas circuit 3 and the 4th gas circuit 4 are in parallel by first gas mixing tube 5, first gas mixing tube 5 and TCD gas
The connection of detector air inlet, TCD detector exhaust outlet are connected to by pipeline with the second triple valve 6, and the second triple valve 6 is in addition
Both ends are separately connected six-way valve and second gas delivery pipe 7, and first gas delivery pipe 103 and second gas delivery pipe 7 pass through the
Two gas mixing tube 8 is in parallel, and second gas mixing tube 8 is connected to the gas access of temperature programming resistance furnace, temperature programming resistance
The gas vent of furnace is connect by pipeline with third triple valve 9, and temperature programming resistance furnace is electrically connected with electrochemical test system, the
The other both ends of three triple valves 9 are separately connected tail gas discharging pipe and third gas delivery pipe, third gas delivery pipe and TCD gas
Another air inlet of detector is connected to, and third gas delivery pipe top is equipped with drying device 12, another row of TCD detector
Port is connected to by pipeline with tail gas discharging pipe；Six-way valve is arranged on pulse gas discharge pipe 102；Pulse air gas handling system with
First gas circuit 1, the second gas circuit 2, third gas circuit 3 and the connection of the 4th gas circuit 4, are used for the first gas circuit 1, the second gas circuit 2, third gas
Road 3 and 4 feed carrier gas of the 4th gas circuit and gas to be measured.
It should be noted that each flowmeter, temperature programming resistance furnace, electrochemical test system in above-mentioned gas air distribution system
(electrochemical workstation), TCD detector are electrically connected with control computer, are passed through and are controlled computer.Wherein four road gases pass through
Corresponding mass flowmenter controls flow, realizes that gas circuit is opened by corresponding check valve and switch valve, passes through and change threeway
The state of valve and switch valve can realize different functions.
Wherein, the first triple valve 101 and the second triple valve 6 can be realized and six-way valve or temperature programming electricity respectively by switching
Furnace is hindered to be connected；Third triple valve 9 can realize into the gas in temperature programming resistance furnace reaction tubes respectively with TCD gas detection
Device is connected with drying device or offgas outlet, and TCD detector is inhaled after entering reaction tube for detection gas by test specimen
The variation of attached amount.And simultaneously, the test specimen in reaction tube in TCD detector is by platinum electrode and electrochemistry
What test macro was connected, the electric signal in gas absorption desorption process is become using electrochemical test system characterization laboratory sample
Change.
Mistake when carrying out test specimen chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization using above-mentioned apparatus
Journey is specific as follows:
1, prepare test specimen
It before test sample, needs to pre-process the test specimen of absorption carrier, general preprocessing process includes
Redox pretreatment and desorption purging.Redox pretreatment is placed in sample in oxidation-reduction quality atmosphere, is handled,
Catalyst sample is mainly carried out redox processing by the process, can also remove carbon distribution, the moisture etc. on sample surfaces.It will
Upper platinum filament is welded on the test specimen surface handled well, and platinum filament is drawn in the reaction tube in temperature programming resistance furnace, with electrochemistry
The upper electrode of test macro is connected.
2, temperature programming is set
Test specimen being put into temperature programming resistance furnace and to resistance furnace temperature programming, resistance furnace is warming up to predetermined temperature,
Temperature program can pass through corresponding resistance furnace program setting on control computer.
3, it selects and opens gas circuit
By pulse air gas handling system, into the first gas circuit 1, feed gas (can be under test gas, be also possible to dilute
Gas), so that gas is led to six-way valve or temperature programming resistance furnace by switching the first triple valve 101, the gas in the first gas circuit 1
Body enters in first gas delivery pipe 103 when flowing to temperature programming resistance furnace, can be realized the pulse drop of gas in the first gas circuit 1
Fixed operation, the specific mistake of pulse titration operation are known as this field routine, just do not do specific introduction herein.When in the first gas circuit 1
Gas when leading to six-way valve, via the second triple valve 6 can with it is any in the second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4
Gas or their gaseous mixture are mixed；Then their gaseous mixture is passed through temperature programming electricity by second gas delivery pipe 7
It hinders in furnace.
It should be noted that at least two-way was passed through in the second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4 is gas to be measured
Body, another way can be carrier gas, be also possible under test gas, when detection, the stream that is passed through by adjusting gas type and gas
Amount can realize the measurement of various mixed gas situations.It should be further noted that pulse air gas handling system is in addition to first
, can also be by other gas circuits, so in the utility model except gas circuit 1, the second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4, arteries and veins
Qi of chong channel ascending adversely gas handling system is not limited only to four road gases, can also be more.Certainly, under normal circumstances, four road gases can meet
Demand.
Specifically, any gas or their gaseous mixture in the second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4, first
It is detected via TCD detector, then under the dilution or immixture of the first gas circuit 1, into temperature programming resistance
Furnace, we access electrochemical test system, select " i-t " or chrono-amperometric function in electrochemical test system, characterization absorption
Carrier carries software automatic collection electric signal to the change in electric in gas absorption desorption process, by electrochemical workstation, leads to
Electric signal parsing chemisorption desorption behavior is crossed, determines adsorption/desorption amount.Meanwhile the gas of temperature programming resistance furnace discharge is again
It is detected, is determined by the front and back variation detected of TCD detector solid in chemical adsorption process by TCD detector
Body surface excess, thus measurement while realizing chemical adsorption amount and chemisorption electric signal.
It should be further noted that the 4th air shooter 10 is also connected on six-way valve, the 4th air shooter 10
One end is connected to six-way valve, and the other end and second gas delivery pipe 7 are connected；4th air shooter 10 and first gas delivery pipe
It is also connected with the 5th air shooter 11 between 103, is also sequentially installed with mass flowmenter and list on the 5th air shooter 11
To valve, switch valve is also equipped in second gas delivery pipe 7.Secondary match can also be realized by above-mentioned setting the utility model
Gas, any gas of the gas that we are passed through using the first gas circuit 1 as carrier gas, in the second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4
Body or their gaseous mixture is under test gas, under test gas are made after TCD detector by the second triple valve 6
Gas mixing in gaseous mixture and the first gas circuit 1 makes under test gas obtain certain times by the carrier gas in the first gas circuit 1
A distribution is completed in several dilutions, and a distribution after dilution is by the switch valve closed in second gas delivery pipe 7, by the
Five air shooters 11 flow to temperature programming resistance furnace, and control stream by the mass flowmenter on the 5th air shooter 11
Amount.
And when needing to carry out secondary distribution, a distribution leads to six-way valve and the first gas by the 4th air shooter 10
Carrier gas in road 1 carries out secondary mixed diluting, is diluted certain multiple again, so that the lower under test gas of concentration is obtained,
Secondary distribution flows to temperature programming resistance furnace by the 5th air shooter 11 again and carries out quantitatively characterizing.As for extension rate, we are logical
It crosses control mass flow to be calculated as determining, the accurate distribution of the minimum achievable 1ppm gas of the device.
In short, gas is conveyed into the first gas circuit, the second gas circuit, third gas circuit and the 4th gas circuit, by corresponding
Switch valve sets the ingredient of gaseous mixture, and sets content by corresponding flow valve, and gaseous mixture is passed through temperature programming electricity
It hinders and carries out adsorption/desorption or reaction in furnace；
4, electro-chemical test
" i-t " or the chrono-amperometric function in electrochemical test system are selected, gas absorption is desorbed in characterization test specimen
Change in electric in the process carries software automatic collection electric signal by electrochemical workstation, parses chemistry by electric signal and inhales
Attached desorption behavior determines adsorption/desorption amount.
It should be noted that being also connected with diluent gas delivery pipe, the diluent gas in above-mentioned second gas delivery pipe 7
Needle valve is installed, for controlling discharge diluent gas on delivery pipe.
Obviously, it is practical without departing from this can to carry out various modification and variations to the utility model by those skilled in the art
Novel spirit and scope.If in this way, these modifications and variations of the present invention belong to the utility model claims and
Within the scope of its equivalent technologies, then the utility model is also intended to include these modifications and variations.Embodiment described above
It is only preferred embodiments for fully illustrating the utility model, protection scope is without being limited thereto.The art
Technical staff made equivalent substitute or transformation on the basis of the utility model, both are within the protection scope of the present invention,
The protection scope of the utility model is subject to claims.
Claims (7)
1. a kind of device that can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization, which is characterized in that packet
Include gas distribution system, pulse air gas handling system, temperature programming resistance furnace, electrochemical test system and TCD detector；
The gas distribution system includes the first gas circuit (1), the second gas circuit (2), third gas circuit (3) and the 4th gas circuit (4), described
First gas circuit (1) connects the first triple valve (101), and in addition both ends are separately connected pulse gas row to first triple valve (101)
Outlet pipe (102) and first gas delivery pipe (103), and mass flowmenter, check valve are sequentially installed in first gas circuit (1)
And switch valve；
Be sequentially installed in second gas circuit (2), third gas circuit (3) and the 4th gas circuit (4) mass flowmenter, check valve and
Switch valve, second gas circuit (2), third gas circuit (3) and the 4th gas circuit (4) are in parallel by first gas mixing tube (5), described
First gas mixing tube (5) is connected to TCD detector air inlet, the TCD detector exhaust outlet by pipeline with
Second triple valve (6) connection, second triple valve (6) are in addition separately connected six-way valve and second gas delivery pipe (7) in both ends,
The first gas delivery pipe (103) and the second gas delivery pipe (7) are in parallel by second gas mixing tube (8), described
Second gas mixing tube (8) is connected to the gas access of temperature programming resistance furnace, the gas vent of described program heating resistance furnace
It is connect by pipeline with third triple valve (9), described program heating resistance furnace is electrically connected with electrochemical test system, the third
The other both ends of triple valve (9) are separately connected tail gas discharging pipe and third gas delivery pipe, the third gas delivery pipe and TCD
Another air inlet of detector is connected to, and third gas delivery pipe top is equipped with drying device (12), the TCD gas
Another exhaust outlet of detector is connected to by pipeline with the tail gas discharging pipe；The six-way valve is arranged in pulse gas discharge pipe
(102) on；
The pulse air gas handling system is connect with the first gas circuit (1), the second gas circuit (2), third gas circuit (3) and the 4th gas circuit (4),
For to the first gas circuit (1), the second gas circuit (2), third gas circuit (3) and the 4th gas circuit (4) feed pulse air.
2. the dress according to claim 1 that can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization
It sets, which is characterized in that further include control computer, each flowmeter, temperature programming resistance furnace, electrochemistry in the gas distribution system
Test macro, TCD detector are electrically connected with control computer.
3. the dress according to claim 1 that can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization
It sets, which is characterized in that diluent gas delivery pipe, the diluent gas discharge are also connected on the second gas delivery pipe (7)
Needle valve is installed on pipe.
4. the dress according to claim 1 that can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization
It sets, which is characterized in that described program heats up, and resistance furnace is interior to be equipped with reaction tube and platinum electrode, and the reaction tube is for placing absorption
Carrier, the platinum electrode are used to connect the electrification outside absorption carrier and described program heating resistance furnace in the reaction tube
Learn test macro.
5. the dress according to claim 1 that can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization
It sets, which is characterized in that the 4th air shooter (10), the 4th air shooter (10) one are also connected on the six-way valve
End is connected to the six-way valve, and the other end and second gas delivery pipe (7) are connected；4th air shooter (10) and described
The 5th air shooter (11) is also connected between first gas delivery pipe (103), on the 5th air shooter (11)
It is sequentially installed with mass flowmenter and check valve, is also equipped with switch valve on the second gas delivery pipe (7).
6. the dress according to claim 4 that can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization
It sets, which is characterized in that the absorption carrier includes catalyst.
7. the dress according to claim 1 that can be realized chemical adsorption amount and chemisorption electric signal simultaneous quantitative characterization
It sets, which is characterized in that it is carrier gas that first gas circuit (1), which is passed through, second gas circuit (2), third gas circuit (3) and the 4th
What at least two-way was passed through in gas circuit (4) is under test gas.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108445090A (en) * | 2018-03-29 | 2018-08-24 | 辽宁科技大学 | Realize device, the method for chemisorption amount and chemisorption electric signal simultaneous quantitative characterization |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108445090A (en) * | 2018-03-29 | 2018-08-24 | 辽宁科技大学 | Realize device, the method for chemisorption amount and chemisorption electric signal simultaneous quantitative characterization |
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