CN108445090A - Realize device, the method for chemisorption amount and chemisorption electric signal simultaneous quantitative characterization - Google Patents
Realize device, the method for chemisorption amount and chemisorption electric signal simultaneous quantitative characterization Download PDFInfo
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Abstract
The invention discloses a kind of devices and methods therefors that can realize chemisorption 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 detectors；Wherein gas distribution system is made of four road gases so that different functions can be achieved by changing the state of triple valve and switch valve in the present apparatus, quantitatively characterizing while to realize chemisorption amount and chemisorption electric signal.Device provided by the invention only characterizes chemical absorption behavior better than traditional chemical adsorption instrument by adsorbance variation；The important information in chemisorption can also be captured by the surface change in electric caused by aerochemistry adsorption process.
Description
Technical field
The present invention relates to a kind of new methods and its device of research chemisorption, in particular for catalyst and its carrier
The detection method and its device of chemisorption.
Background technology
Heterogeneous catalysis process is to convert reactant molecule to reaction product by the cycle 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
Soon, 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 for the 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, people using various modern spectroscopy technique and with conventional characterization
Means are combined, 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, this important sphere of learning of formation 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
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 includes mainly temperature programmed desorption (TPD), program liter
Temperature reduction (TPR), temperature programmed oxidation (TPO), temperature programmed surface reaction (TPSR).It is urged in research by temperature-programmed technique
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 lived
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 it is characterized in there are one important during chemisorption：Adsorption molecule is sent out with surface of solids atom (or molecule)
The transfer of raw electronics is exchanged or is shared, and forms the absorption of sorption chemical key.Since there are the uneven field of force, surfaces for the surface of solids
On atom often also have 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
To study a kind of new method of chemisorption.Therefore it provides a kind of measuring surface of solids adsorbance during chemisorption simultaneously
Variation with the electric signal of gas sensing is necessary come the method and apparatus for capturing chemisorption information.
Invention content
In order to solve the deficiencies in the prior art, the present invention provides a kind of new methods and its dress for characterizing chemisorption
It sets, the variation of surface of solids adsorbance and electric signal caused in particular solid surface process can be adsorbed on detection gas,
So as to which chemical absorption behavior is inferred and characterized by the variation of adsorbance and absorption electric signal simultaneously.
The present invention provides it is a kind of can realize chemisorption 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 TCD detectors；
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 it is sequentially installed with mass flowmenter, check valve and switch valve in first gas circuit；
It is sequentially installed with mass flowmenter, check valve and switch 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
TCD detector air inlets are connected to, and the TCD detectors 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, the third gas delivery pipe is sent to be connected to another air inlet of TCD detectors, and in the third gas delivery pipe
Portion is equipped with drying device, and another exhaust outlet of TCD detectors 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 is connect with the first gas circuit, the second gas circuit, third gas circuit and the 4th gas circuit, 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 controlling computer, each flowmeter, temperature programming resistance in the gas distribution system
Stove, electrochemical test system, TCD detectors are electrically connected with control computer.
Preferably, diluent gas delivery pipe, the diluent gas delivery pipe are also associated 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 absorption carrier in the reaction tube and the electricity outside described program heating resistance furnace
Test chemical system.
Preferably, the 4th air shooter, described 4th air shooter one end and institute are also associated on the six-way valve
Six-way valve connection is stated, the other end is connected with second gas delivery pipe；4th air shooter and first gas conveying
It is also associated 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.
The present invention also provides realize chemisorption amount and chemisorption electric signal simultaneous quantitative characterization using above-mentioned apparatus
Method, include the following steps：
S1：Absorption carrier is put into described program heating resistance furnace, is connected by platinum electrode and electrochemical test system
It connects, described program heating resistance furnace progress temperature programming is controlled to predetermined temperature by controlling computer；
S2：By pulse air gas handling system into the first gas circuit feed gas, keep gas logical by switching the first triple valve
To six-way valve or temperature programming resistance furnace, temperature programming is flowed to when the gas in the first gas circuit enters in first gas delivery pipe
When resistance furnace, the pulse titration operation of gas in the first gas circuit can be realized；When the gas in the first gas circuit leads to six-way valve,
It can be carried out with any gas in the second gas circuit, third gas circuit and the 4th gas circuit or their gaseous mixture via the second triple valve
Mixing；
S3：Second gas circuit, third gas circuit and any gas in the 4th gas circuit or their gaseous mixture are through TCD gases
After detector, lead to temperature programming resistance furnace after making the gas mixing in gaseous mixture and the first gas circuit by the second triple valve, or
Lead to six-way valve after making the gas mixing in gaseous mixture and the first gas circuit by the second triple valve, with the gas in the first gas circuit into
The secondary mixed diluting of row, realizes secondary distribution；
It is supplied gas body by least a-road-through of the pulse air gas handling system into the second gas circuit, third gas circuit and the 4th gas circuit,
The ingredient of gaseous mixture is set by corresponding switch valve, and flow is set by corresponding flow valve, by gaseous mixture
It is passed through in temperature programming resistance furnace and carries out adsorption/desorption or reaction；The front and back variation detected by TCD detectors is true
Determine chemisorption amount；
S4：Select " i-t " or the chrono-amperometric function in electrochemical test system, characterization absorption carrier de- to gas absorption
Change in electric during attached carries software automatic collection chemisorption electric signal by electrochemical workstation, is inhaled by chemistry
Attached electric signal parses chemisorption desorption behavior.
Compared with prior art, the beneficial effects of the present invention are：
Gas distribution system in device provided by the invention is made of four road gases so that the present apparatus can pass through change
Different functions can be achieved in the state of triple valve, six-way valve and switch valve, to realize chemisorption amount and chemisorption electricity
Quantitatively characterizing while signal.Device provided by the invention is better than traditional chemical adsorption instrument only by adsorbance variation come characterization
Learn absorption behavior；It can also be captured in chemisorption by the surface change in electric caused by aerochemistry adsorption process
Important information.In addition, device provided by the invention is better than the common level-one air distribution system of traditional chemical adsorption instrument, it can be real
Existing two level distribution, the accurate distribution of minimum achievable 1ppm gases.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 can realize chemisorption amount and chemisorption electric signal simultaneous quantitative characterization to be provided in an embodiment of the present invention
Device schematic diagram；
Fig. 2 is a concentration H2It is passed through resistance furnace by different order with b concentration Cs O, test specimen encounters the electric signal after gas
Change curve；
Fig. 3 is a concentration H2After respectively reaching same resistance value with b concentration Cs O, then it is passed through c concentration H2Change in electric afterwards；
Fig. 4 is H2The adsorption process change in electric curve in different carrier gas；
Fig. 5 is H2The adsorption process n values in different carrier gas.
Specific implementation mode
In order to enable those skilled in the art to more fully understand, technical scheme of the present invention is practiced, with reference to specific
The invention will be further described for embodiment, but illustrated embodiment is not as a limitation of the invention.
Unless otherwise defined, the hereinafter used all technical terms for being and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
The device provided by the invention that can realize chemisorption amount and chemisorption electric signal simultaneous quantitative characterization, specifically
As shown in Figure 1, including 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
It is carrier gas to send, and the first gas circuit 1 connects the first triple valve 101, and first triple valve, 101 other both ends are separately connected arteries and veins
Gas outlet pipe 102 and first gas delivery pipe 103 are rushed, and mass flowmenter, check valve are sequentially installed in the first gas circuit 1
And switch valve；It is sequentially installed with mass flowmenter, check valve and switch in second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4
Valve, the second gas circuit 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 with
TCD detector air inlets are connected to, and TCD detectors exhaust outlet is connected to by pipeline with the second triple valve 6, the second threeway
6 other both ends of valve are separately connected six-way valve and second gas delivery pipe 7, first gas delivery pipe 103 and second gas delivery pipe 7
In parallel by second gas mixing tube 8, second gas mixing tube 8 is connected to the gas access of temperature programming resistance furnace, program liter
The gas vent of warm resistance furnace is connect by pipeline with third triple valve 9, temperature programming resistance furnace and electrochemical test system electricity
Connection, the other both ends of third triple valve 9 are separately connected tail gas discharging pipe and third gas delivery pipe, third gas delivery pipe with
Another air inlet of TCD detectors is connected to, and third gas delivery pipe top is equipped with drying device 12, TCD gas detections
Another exhaust outlet of device is connected to by pipeline with tail gas discharging pipe；Six-way valve is arranged on pulse gas discharge pipe 102；Pulse air into
Gas system is connect with the first gas circuit 1, the second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4, is used for the first gas circuit 1, the second gas circuit
2, third gas circuit 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 detectors 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
Stove 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 detections
Device is connected with drying device or offgas outlet, and TCD detectors are 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 detectors is by platinum electrode and electrochemistry
Test system is connected, and characterizing laboratory sample using electrochemical test system becomes the electric signal in gas absorption desorption process
Change.
Mistake when carrying out test specimen chemisorption 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 pre-processes and desorption purging.Redox pretreatment is that sample is placed 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
Platinum filament in the test specimen surface soldered handled well, platinum filament are drawn in the reaction tube in temperature programming resistance furnace, with electrochemistry
The upper electrode of test system is connected.
2, temperature programming is set
Test specimen is put into temperature programming resistance furnace and to resistance furnace temperature programming, resistance furnace is warming up to predetermined temperature,
Temperature program can be by controlling corresponding resistance furnace program setting on 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, can also be dilution
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 realize the pulse drop of gas in the first gas circuit 1
The specific mistake of fixed operation, pulse titration operation is known as this field routine, does not just 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 stove.
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, can also be 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 present invention except gas circuit 1, the second gas circuit 2, third gas circuit 3 and the 4th gas circuit 4, pulse air
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 detectors, then under the dilution of the first gas circuit 1 or immixture, into temperature programming resistance
Stove, 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 that TCD detectors are detected solid in chemical adsorption process by TCD detectors
Body surface excess, to be measured while realizing chemisorption amount and chemisorption electric signal.
It should be further noted that the 4th air shooter 10 is also associated on six-way valve, the 4th air shooter 10
One end is connected to six-way valve, and the other end is connected with second gas delivery pipe 7；4th air shooter 10 and first gas delivery pipe
It is also associated with the 5th air shooter 11 between 103, mass flowmenter and list are also sequentially installed on the 5th air shooter 11
To valve, switch valve is also equipped in second gas delivery pipe 7.Secondary distribution can also be realized by the above-mentioned setting present invention, I
The gas that is passed through using the first gas circuit 1 as carrier gas, the second gas circuit 2, third gas circuit 3 and any gas in the 4th gas circuit 4 or
Be their gaseous mixture be under test gas for, under test gas makes mixing after TCD detectors, by the second triple valve 6
Gas mixing in gas and the first gas circuit 1 makes under test gas obtain certain multiple by the carrier gas in the first gas circuit 1
A distribution is completed in dilution, and a distribution after dilution is by closing the switch valve in second gas delivery pipe 7, by the 5th gas
Body delivery pipe 11 flows to temperature programming resistance furnace, and controls flow by the mass flowmenter on the 5th air shooter 11.
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, to obtain the lower under test gas of concentration,
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 gases 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 stove；
4, electro-chemical test
Select " i-t " or the chrono-amperometric function in electrochemical test system, characterization test specimen that gas absorption is desorbed
Change in electric in the process carries software automatic collection electric signal by electrochemical workstation, and parsing chemistry by electric signal inhales
Attached desorption behavior determines adsorption/desorption amount.
It should be noted that being also associated 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.
We are specifically illustrated with regard to device and method provided in an embodiment of the present invention below.
(1) gas with various is passed through resistance furnace by different order, and test specimen encounters the change in electric after gas
First, a concentration H is passed through by the second gas circuit 22；On this basis, the second triple valve 6 turns to second gas conveying
Pipe 7, then b concentration C O are passed through by third gas circuit 3, two-way gas successively enters temperature programming resistance furnace via TCD detectors
In, it is tested by electrochemical test system, after electric current reaches balance, while removing a concentration H2With b concentration C O, material current
Value is restored to ground state.Second, ventilation sequence with it is previous opposite.Gas with various is passed through resistance furnace, test specimen by different order
It is as shown in Figure 2 to encounter the change in electric Dependence Results after gas, it can be seen that, a concentration H2With the ventilation of b concentration Cs O sequence with
It is previous on the contrary, still the current value of final sensitive material is as before, this shows CO and H2The end-state of eutectoid content and suction
Attached sequence is unrelated, meanwhile, show that the absorption of the two is mono layer adsorption.Because if the adsorption process belongs to polymolecular layer suction
It is attached, then CO and H2Adsorbed layer structure difference can occur because absorption sequence is different, to which different electric signals should be shown.Cause
This, the adsorbed state of gas can be speculated by gas sensing behavior.This is traditional chemical adsorption instrument only by chemisorption amount
The absorption information that can not be captured.
(2) after gas with various respectively reaches same resistance value, then it is passed through the change in electric after same gas
First, a concentration H is passed through by the second gas circuit 22；On this basis, the second triple valve 6 turns to second gas conveying
Pipe 7, then b concentration C O are passed through by third gas circuit 3, it is passed through c concentration H after electric current reaches balance, then in the 4th gas circuit 42, pass through electricity
The response of test chemical system testing, generation changes and differs, respectively Δ A and Δ B, specifically as shown in figure 3, this says
It is bright, CO and H2Between exist interaction.Therefore, when can deduce multicomponent gas eutectoid content by gas sensing behavior,
Interaction between them.This is the absorption information that traditional chemical adsorption instrument can not only be captured by chemisorption amount.
(3) under the conditions of different carrier gas, the H of isoconcentration gradient2Specimen surface of the gas absorption caused by specimen surface
The variation of electric signal
90%H is measured using device provided by the invention respectively2+ 10%O2, 80%H2+ 20%O2, 70%H2+ 30%O2、
60%H2+ 40%O2, 40%H2+ 60%O2, 20%H2+ 80%O2Under the conditions of carrier gas, the H of isoconcentration gradient2It is adsorbed on sample table
The case where specimen surface electric signal caused by face, first, the H of various concentration is passed through by the second gas circuit 22；On this basis,
Second triple valve 6 turns to second gas delivery pipe 7, then the O of corresponding concentration is passed through by third gas circuit 32, pass through electro-chemical test system
Unified test tries, H2The adsorption process change in electric situation in different carrier gas, obtained H2The adsorption process electric signal in different carrier gas
Change curve by obtained curve as shown in figure 4, utilize empirical formula R=1+kCnFit response and pure gas
The quantitative relationship equation of concentration.Formula both sides take logarithm that can obtain n values, H2Adsorption process n values such as Fig. 5 institutes in different carrier gas
Show.In formula, response R is the resistance variations multiple of value laboratory sample, H2Concentration is indicated with C.It can be found that in n values and carrier gas
Oxygen concentration relationship is little, this illustrates O2Adsorption potential and H2It differs.
(4) level-one distribution and two level distribution
First, it is passed through the carrier gas of atm number by the first gas circuit 1, a concentration H is passed through by the second gas circuit 22, adjust six
The flow direction of port valve makes a concentration H by the second triple valve 62It is mixed with the carrier gas in the first gas circuit 1, by the first gas circuit 1
Carrier gas, so that under test gas has been obtained the dilution of certain multiple, complete a distribution.A concentration H after dilution2Pass through the 4th
Air shooter 10 leads to six-way valve, and secondary mixed diluting is carried out with the carrier gas in the first gas circuit 1, is diluted certain times again
Number, to obtain the lower H of concentration2, to realize H2Secondary distribution, as extension rate, we pass through mass flowmenter
For determination, the accurate distribution of the minimum achievable 1ppm gases of the device.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.Embodiment described above is only to absolutely prove the present invention
And the preferred embodiment lifted, protection domain are without being limited thereto.Those skilled in the art institute on the basis of the present invention
The equivalent substitute of work or transformation, within protection scope of the present invention, protection scope of the present invention is subject to claims.
Claims (8)
1. a kind of device that can realize chemisorption 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 detectors；
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 it is sequentially installed with mass flowmenter, check valve 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 described by first gas mixing tube (5) parallel connection
First gas mixing tube (5) is connected to TCD detector air inlets, the TCD detectors exhaust outlet by pipeline with
Second triple valve (6) is connected to, and second triple valve (6) is 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 described by second gas mixing tube (8) parallel connection
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 with third triple valve (9) by pipeline, 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 realize chemisorption amount and chemisorption electric signal simultaneous quantitative characterization
It sets, which is characterized in that further include controlling computer, each flowmeter, temperature programming resistance furnace, electrochemistry in the gas distribution system
Test system, TCD detectors are electrically connected with control computer.
3. the dress according to claim 1 that can realize chemisorption 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 associated on the second gas delivery pipe (7)
Needle valve is installed on pipe.
4. the dress according to claim 1 that can realize chemisorption 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 adsorbed for placing
Carrier, the platinum electrode are used to connect the absorption carrier in the reaction tube and the electrification outside described program heating resistance furnace
Learn test system.
5. the dress according to claim 1 that can realize chemisorption 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 associated on the six-way valve
End is connected to the six-way valve, and the other end is connected with second gas delivery pipe (7)；4th air shooter (10) and described
The 5th air shooter (11) is also associated between first gas delivery pipe (103), on the 5th air shooter (11)
It is sequentially installed with mass flowmenter and check valve, switch valve is also equipped on the second gas delivery pipe (7).
6. the dress according to claim 1 that can realize chemisorption 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 realize chemisorption 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.
8. a kind of side realizing chemisorption amount and chemisorption electric signal simultaneous quantitative characterization using claim 1 described device
Method, which is characterized in that include the following steps：
S1：Absorption carrier is put into described program heating resistance furnace, is connect, is led to electrochemical test system by platinum electrode
It crosses control computer control described program heating resistance furnace and carries out temperature programming to predetermined temperature；
S2：By pulse air gas handling system into the first gas circuit (1) feed gas, by switch the first triple valve (101) make gas
Body leads to six-way valve or temperature programming resistance furnace, when the gas in the first gas circuit (1) enters in first gas delivery pipe (103)
When flowing to temperature programming resistance furnace, the pulse titration operation of gas in the first gas circuit (1) can be realized；When in the first gas circuit (1)
Gas when leading to six-way valve, can be with the second gas circuit (2), third gas circuit (3) and the 4th gas circuit via the second triple valve (6)
(4) any gas or their gaseous mixture are mixed in；
S3：Second gas circuit (2), third gas circuit (3) and any gas in the 4th gas circuit (4) or their gaseous mixture are through TCD
After detector, lead to temperature programming after making the gas mixing in gaseous mixture and the first gas circuit (1) by the second triple valve (6)
Resistance furnace, or lead to six-way valve after making the gas mixing in gaseous mixture and the first gas circuit (1) by the second triple valve (6), with
Gas in one gas circuit (1) carries out secondary mixed diluting, realizes secondary distribution；
Pass through pulse air gas handling system being at least passed through all the way into the second gas circuit (2), third gas circuit (3) and the 4th gas circuit (4)
Gas is set the ingredient of gaseous mixture by corresponding switch valve, and sets flow by corresponding flow valve, will be mixed
It closes gas and is passed through progress adsorption/desorption or reaction in temperature programming resistance furnace；The front and back change detected by TCD detectors
Change and determines chemical adsorbance；
S4：Select " i-t " or the chrono-amperometric function in electrochemical test system, characterization absorption carrier that gas absorption was desorbed
Change in electric in journey carries software automatic collection chemisorption electric signal by electrochemical workstation, passes through chemisorption electricity
Signal resolution chemisorption desorption behavior.
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| CN2610324Y (en) * | 2003-03-10 | 2004-04-07 | 中国石油化工股份有限公司 | Catalyst properties weight adsorption measuring device |
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