CN105067752A - Program heating analysis equipment and method for testing property of its catalyst - Google Patents
Program heating analysis equipment and method for testing property of its catalyst Download PDFInfo
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- CN105067752A CN105067752A CN201510446854.7A CN201510446854A CN105067752A CN 105067752 A CN105067752 A CN 105067752A CN 201510446854 A CN201510446854 A CN 201510446854A CN 105067752 A CN105067752 A CN 105067752A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 67
- 238000012360 testing method Methods 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 54
- 230000009467 reduction Effects 0.000 claims abstract description 34
- 238000012545 processing Methods 0.000 claims abstract description 25
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 23
- 238000003795 desorption Methods 0.000 claims abstract description 21
- 230000003647 oxidation Effects 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000010926 purge Methods 0.000 claims description 44
- 238000006722 reduction reaction Methods 0.000 claims description 42
- 238000001514 detection method Methods 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000004375 physisorption Methods 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000009830 intercalation Methods 0.000 claims description 3
- 230000002687 intercalation Effects 0.000 claims description 3
- 238000007781 pre-processing Methods 0.000 claims description 2
- 230000005619 thermoelectricity Effects 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 4
- 230000006835 compression Effects 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- 230000002468 redox effect Effects 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002638 heterogeneous catalyst Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007172 homogeneous catalysis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
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Abstract
The invention provides a program heating analysis equipment and a method for testing property of its catalyst, which can be used for testing program heating reduction, program heating oxidation and temperature programmed desorption. The program heating analysis equipment comprises a first air supply pipeline, a second air supply pipeline, a pressure-reducing valve, a pressure-stabilizing valve, a constant flow valve, a compression gauge, a mass flowmenter, a non return valve, a six-way valve, a U-shaped reaction tube, heating furnaces, a thermocouple, a temperature controller, a thermal conductance pool detector, a data processing work station and a computer. The design of the six-way valve can conveniently realize the switching of two ways of gas, a purpose of simultaneous operation of a pretreatment process of a catalyst sample and a base line recording process of the equipment can be reached, time is greatly saved, and testing efficiency is increased; design of three heating furnaces is convenient for replacing the high temperature heating furnace, waiting time for cooling the heating furnace is saved, and testing efficiency is increased.
Description
Technical field
The invention belongs to vapor solid catalysis technical field, particularly a kind of property detection method of temperature programme analytical equipment and catalyzer thereof, be mainly used in the redox property and surface acidic-basic property etc. of detecting catalyst sample.
Background technology
As everyone knows, the chemical industry of more than 80% relates to catalytic process, and the development level of catalysis technique has reacted national development degree.Meanwhile, catalysis technique also plays very important effect in the fields such as environmental pollution improvement, new energy development and new material development.Catalytic reaction, according to the similarities and differences of physical state, can be divided into: homogeneous catalysis and heterogeneous catalyst.Wherein, heterogeneous catalyst becomes the focus of research owing to having the advantages such as separation is simple, catalyzer is reusable.Vapor solid catalysis is typical heterogeneous catalyst, plays very important role at environment and energy field, and especially in today that environmental pollution and energy scarcity aggravate, its importance is more obvious.
The redox property of catalyst sample and surface acidic-basic property can its catalytic performances in gas-solid-phase catalytic reaction of appreciable impact, thus become the important regulating and controlling index that researcher optimizes existing catalyzer and initiative new catalyst.The great interest of how simply, the data such as redox property and surface acidic-basic property obtaining catalyst sample efficiently cause catalyst operation person.Under catalyst sample being exposed to specific gas condition, carrying out temperature programme and record corresponding data, then to data analysis, effectively can obtain the information such as redox property and surface acidic-basic property of catalyst sample.Therefore, instrument development personnel are devoted to the research and development of related equipment always.
At present, although both at home and abroad more existing companies have developed the test of temperature programme analytical equipment for the redox property of catalyst sample and surface acidic-basic property etc.But all there is a common fault---testing efficiency is too low: the pre-service (purging) of catalyst sample and instrument are walked baseline two steps and can not synchronously be carried out; Need again to walk baseline before each catalyst sample test; Heating furnace is non-dismountable, and slowly, this greatly reduces the efficiency of researcher in cooling.
Summary of the invention
The deficiencies in the prior art in view of the above, the object of the present invention is to provide a kind of can be used for catalyst sample redox property and simple, the efficient temperature programme analytical equipment of test and the property detection method of catalyzer thereof such as surface acidic-basic property, walking baseline step and can carrying out simultaneously of pre-service (purging) process of catalyst sample and instrument, saves time, promotes testing efficiency.
For achieving the above object and other relevant objects, the invention provides a kind of temperature programme analytical equipment, test for temperature programmed reduction, temperature programmed oxidation and temperature programmed desorption, comprise the first supply air line, the second supply air line, reactor, heating arrangement, thermal conductivity cell detector and six-way valve, described first supply air line is connected with the first interface of six-way valve, second supply air line is connected with the 3rd interface of six-way valve by after the first side gas circuit of thermal conductivity cell detector, emptying after the 4th interface of six-way valve connects the second side gas circuit of thermal conductivity cell detector by the road; Described reactor is arranged in heating arrangement, and the air intake opening of reactor and gas outlet are connected respectively by the second interface of pipeline and six-way valve and the 5th interface, and the 6th interface of described six-way valve is emptying.
As preferably: described first supply air line and the second supply air line include the gas cylinder, reduction valve, pressure maintaining valve, permanent flow valve, tensimeter, mass flowmeter and the retaining valve that are successively set on gas circuit pipeline, the described retaining valve of the first supply air line is connected with the first interface of six-way valve, and the retaining valve of described second supply air line is connected with the first side gas circuit of thermal conductivity cell detector.
As preferably: also comprise data processing stations and computer, described data processing stations is connected with thermal conductivity cell detector and computer respectively, carries out data processing and transmission.
As preferably: also comprise detector unit and temperature controller, the beds in described detector unit intercalation reaction device, and be connected with temperature controller, described temperature controller is connected with heating arrangement.
As preferably: described detector unit is thermoelectricity occasionally temperature sensor.
As preferably: described reactor is U-shaped reaction tube, and described heating arrangement is plug-in type heating furnace, comprise a work heating furnace and at least one supplementary heater.
As preferably: described first purge gas is high-purity N
2, described first reacting gas is H
2/ N
2or CO/He combination gas, described second reacting gas is O
2/ N
2combination gas, described second purge gas is high-purity He, and described 3rd reacting gas is NH
3/ He combination gas, CO
2/ He combination gas, SO
2/ He combination gas, NO/He combination gas or O
2/ He combination gas.
The present invention also provides a kind of property detection method of catalyzer simultaneously, comprises temperature programmed reduction test, temperature programmed oxidation test and temperature programmed desorption test, also comprises described temperature programme analytical equipment;
Described temperature programmed reduction test is: the first purge gas purges catalyst sample at a set temperature through the first supply air line; After being down to room temperature, switch six-way valve and make the first supply air line emptying through the 6th interface, the first reacting gas flows through beds through the second supply air line, and temperature programme makes the first reacting gas and catalyst sample generation reduction reaction; Then the first reacting gas signal is detected with thermal conductivity cell detector; Gather thermal conductivity cell detector data by data processing stations, intuitively show finally by computer.
Described temperature programmed oxidation test is: after the reduction reaction of said procedure heating reduction test completes and is down to room temperature, first reacting gas is switched to the second reacting gas, and temperature programme makes the second reacting gas and the catalyst sample generation oxidation reaction be reduced; Then the second reacting gas signal is detected with thermal conductivity cell detector; Gather thermal conductivity cell detector data by data processing stations, intuitively show finally by computer.
Described temperature programmed desorption test is: the second purge gas purges catalyst sample at a set temperature through the second supply air line; After being down to 100 DEG C, switch six-way valve, the 3rd reacting gas passes into through the first supply air line and makes catalyst sample absorption saturated; Again switch six-way valve, the second purge gas is again after the second supply air line passes into and purges catalyst sample physisorption thing, and the second side gas circuit through thermal conductivity cell detector is emptying; Temperature programme makes catalyst sample chemical absorption of surface species generation desorption, detects desorbed species signal with thermal conductivity cell detector; Gather thermal conductivity cell detector data with data processing stations, intuitively show finally by computer.
As preferably: in described temperature programmed reduction test, the walking baseline and can carry out simultaneously of the preprocessing process of catalyst sample and instrument: the first purge gas is when the first supply air line purges catalyst sample, entered the second side gas circuit of thermal conductivity cell detector after first reacting gas can flow through the first side gas circuit of thermal conductivity cell detector by six-way valve, thermal conductivity cell detector is normally worked, instrument normally walks baseline.
As preferably: described first purge gas is high-purity N
2, described first reacting gas is H
2/ N
2or CO/He combination gas, described second reacting gas is O
2/ N
2combination gas, described second purge gas is high-purity He, and described 3rd reacting gas is NH
3/ He combination gas, CO
2/ He combination gas, SO
2/ He combination gas, NO/He combination gas or O
2/ He combination gas.
Principle of work of the present invention is as follows:
This temperature programme analytical equipment can be used for the tests such as temperature programmed reduction, temperature programmed oxidation and temperature programmed desorption.For temperature programmed reduction, its principle is: high-purity N
2catalyst sample is purged at a certain temperature, so that clean catalysis agent sample surfaces by the first supply air line; After being down to room temperature, H
2/ N
2(or CO/He) combination gas flows through beds by the second supply air line; Temperature programme makes H
2or CO and catalyst sample generation reduction reaction, detect H with thermal conductivity cell detector
2or CO signal; Gather thermal conductivity cell detector data with data processing stations again, intuitively show finally by computer.For temperature programmed oxidation, its principle is: high-purity N
2catalyst sample is purged at a certain temperature, so that clean catalysis agent sample surfaces by the first supply air line; After being down to room temperature, H
2/ N
2combination gas flows through beds by the second supply air line; Temperature programme makes H
2with catalyst sample generation reduction reaction; After being down to room temperature, by H
2/ N
2combination gas switches to O
2/ N
2combination gas, temperature programme makes O
2catalyst sample generation oxidation reaction with being reduced, detects O with thermal conductivity cell detector
2signal; Gather thermal conductivity cell detector data with data processing stations again, intuitively show finally by computer.For temperature programmed desorption, its principle is: high-purity He purges catalyst sample at a certain temperature by the second supply air line, so that clean catalysis agent sample surfaces; After being down to 100 DEG C, NH
3/ He (or CO
2/ He or SO
2/ He or NO/He or O
2/ He) combination gas by the first supply air line flow through beds make catalyst sample adsorb saturated, physisorption residual gas is blown off at this temperature with high-purity He, temperature programme makes catalyst sample chemical absorption of surface species generation desorption, detects desorbed species signal with thermal conductivity cell detector; Gather thermal conductivity cell detector data with data processing stations again, intuitively show finally by computer.It should be noted that high-purity N
2be the purity range can determined in prior art with high-purity He.
As mentioned above, the invention has the beneficial effects as follows:
1. by introducing the design of six-way valve, the switching of two-way gas can be realized easily, walk with what reach pre-service (purging) process of catalyst sample and instrument the object that baseline step can carry out simultaneously, greatly save the time, improve testing efficiency;
2. by introducing the design of plug-in heating furnace, being equipped with multiple plug-in heating furnace, facilitating the replacing of high-temperature heater, save the stand-by period of heating furnace cooling, improve testing efficiency;
3. material requested is general is easy to get; Simple, convenient, to tester without particular/special requirement; Energy consumption is low, and efficiency is high; There is significant application prospect.
Accompanying drawing explanation
Fig. 1 is the fundamental diagram of temperature programme analytical equipment involved in the present invention;
Fig. 2 is the temperature programmed reduction test comparison collection of illustrative plates of temperature programme analytical equipment involved in the present invention and other company's like product;
Fig. 3 is the temperature programmed oxidation test comparison collection of illustrative plates of temperature programme analytical equipment involved in the present invention and other company's like product;
Fig. 4 is the temperature programmed desorption test comparison collection of illustrative plates of temperature programme analytical equipment involved in the present invention and other company's like product.
Piece mark explanation
1,2: gas cylinder; 3: reduction valve; 4: pressure maintaining valve; 5: permanent flow valve; 6: tensimeter; 7: mass flowmeter; 8: retaining valve; 9: six-way valve; 10:U type reaction tube; 11: heating furnace; 12: thermopair; 13: sample; 14: temperature controller; 15: thermal conductivity cell detector; 16: data processing stations; 17: computer.
Embodiment
By particular specific embodiment, embodiments of the present invention are described below, person skilled in the art scholar the content disclosed by this instructions can understand other advantages of the present invention and effect easily.
As shown in Figure 1, a kind of temperature programme analytical equipment, test for temperature programmed reduction, temperature programmed oxidation and temperature programmed desorption, comprise the first supply air line, the second supply air line, six-way valve 9, U-shaped reaction tube 10, heating arrangement, thermal conductivity cell detector 15, data processing stations 16 and computer 17, in diagram, six-way valve 9 is followed successively by first interface, the second interface, the 3rd interface, the 4th interface, the 5th interface and the 6th interface in the counterclockwise direction; First supply air line is connected with the first interface of six-way valve 9, second supply air line connects the first side gas circuit of thermal conductivity cell detector 15 by pipeline, first side gas circuit is connected with the 3rd interface of six-way valve 9 by pipeline, 4th interface of six-way valve 9 connects the second side gas circuit of thermal conductivity cell detector 15 by the road, and the second side gas circuit is emptying; U-shaped reaction tube 10 is arranged in heating arrangement, and the air intake opening of U-shaped reaction tube 10 is connected with the second interface of six-way valve 9 by pipeline, and the gas outlet of U-shaped reaction tube 10 is connected with the 5th interface by pipeline, and the 6th interface of six-way valve 9 is emptying.Described first supply air line and the second supply air line include the gas cylinder 1 and 2, reduction valve 3, pressure maintaining valve 4, permanent flow valve 5, tensimeter 6, mass flowmeter 7 and the retaining valve 8 that are successively set on gas circuit pipeline, the retaining valve 8 of the first supply air line is connected with the first interface of six-way valve 9, and the retaining valve 8 of the second supply air line is connected with the first side gas circuit of thermal conductivity cell detector 15.
Described data processing stations 16 is connected with thermal conductivity cell detector 15 and computer 17 respectively, carries out data processing and transmission.For the ease of controlling U-shaped reaction tube 10 interior reaction temperature, be also provided with detector unit and temperature controller 14, the beds in detector unit intercalation reaction device, and be connected with temperature controller 14, temperature controller 14 is connected with heating arrangement.
In this example, detector unit is thermopair 12.In order to improve testing efficiency, reduce heating furnace 11 and lower the temperature the stand-by period, heating arrangement is plug-in type heating furnace 11, comprises a work heating furnace and 2 supplementary heaters, to switch.
The direction of arrow shown in Fig. 1 is gas flow direction, in this example the first supply air line gas cylinder 1 in be gas A, be gas B in the gas cylinder 2 of the second supply air line, through reduction valve 3 controlled pressure after gas A derives from gas cylinder 1, flow through pressure and the steady air current that gas A guaranteed by pressure maintaining valve 4 and permanent flow valve 5 again, then an external tensimeter 6 detects actual pressure, next the flow of gas A is accurately controlled by mass flowmeter 7, being connected in series a retaining valve 8 again avoids other gas backwash to damage mass flowmeter 7, the flow direction of gas A is controlled finally by a six-way valve 9, as shown in Figure 1, enter U-shaped reaction tube 10 through dotted line pipeline (first interface is to the second interface) to contact with catalyst sample 13, directly emptying through solid line pipeline (first interface is to the 6th interface).Through reduction valve 3 controlled pressure after gas B derives from gas cylinder 2, flow through pressure and the steady air current that gas B guaranteed by pressure maintaining valve 4 and permanent flow valve 5 again, then an external tensimeter 6 detects actual pressure, next the flow of gas B is accurately controlled by mass flowmeter 7, being connected in series a retaining valve 8 again avoids other gas backwash to damage mass flowmeter 7, controlled the flow direction of gas B by six-way valve 9 after last gas B flows through the first side gas circuit of thermal conductivity cell detector 15, as shown in Figure 1, it is emptying after dotted line pipeline (the 3rd interface is to the 4th interface) directly enters the second side gas circuit of thermal conductivity cell detector 15, enter U-shaped reaction tube 10 through solid line pipeline (the 3rd interface is to the second interface) to contact with catalyst sample 13, emptying after then flowing through the second side gas circuit of thermal conductivity cell detector 15.Temperature Programmed Processes controls mainly through temperature controller 14, thermopair 12 and heating furnace 11.Thermopair 12 detects the temperature feedback of beds to temperature controller 14, and temperature controller 14 sends signal control heating furnace 11 according to the heating schedule of setting and heats up, to realize the object of temperature programme.Gas signal in Temperature Programmed Processes, after thermal conductivity cell detector 15 detects, gathers corresponding data by data processing stations 16, intuitively shows finally by computer 17.
Equipment involved in the present invention is when gas A carries out pre-service (purging) to catalyst sample 13, the second side gas circuit of thermal conductivity cell detector 15 is entered by the dotted line pipeline of six-way valve 9, to guarantee that thermal conductivity cell detector 15 can normally work, instrument normally can walk baseline after gas B can flow through the first side gas circuit of thermal conductivity cell detector 15.That is, the walking baseline step and can carry out simultaneously of pre-service (purging) process of catalyst sample 13 and instrument, avoid the drawback that these two steps of other company's like product must be carried out separately, this greatly saves the time, improves testing efficiency.In addition, equipment configuration involved in the present invention has 3 plug-in heating furnaces, after completing each heating steps, all the heating furnace being in the condition of high temperature can be taken off, change the heating furnace being in room temperature, carry out follow-up heating process, efficiently avoid the fixed heating furnace of other company's like product and to lower the temperature slow shortcoming, this greatly save heating furnace cooling stand-by period, improve testing efficiency.
The present invention also provides a kind of property detection method of the catalyzer based on said procedure intensification analytical equipment simultaneously, comprises temperature programmed reduction test, temperature programmed oxidation test and temperature programmed desorption method of testing.
Described temperature programmed reduction test is: the first purge gas purges catalyst sample 13 at a set temperature through the first supply air line; After being down to room temperature, switch six-way valve 9 and make the first supply air line emptying through the 6th interface, the first reacting gas flows through beds through the second supply air line, and temperature programme makes the first reacting gas and catalyst sample 13 that reduction reaction occur; Then the first reacting gas signal is detected with thermal conductivity cell detector 15; Gather thermal conductivity cell detector 15 data by data processing stations 16, intuitively show finally by computer 17.
Described temperature programmed oxidation test is: after the reduction reaction of said procedure heating reduction test completes and is down to room temperature, first reacting gas is switched to the second reacting gas, and temperature programme makes the second reacting gas, with the catalyst sample 13 be reduced, oxidation reaction occur; Then the second reacting gas signal is detected with thermal conductivity cell detector 15; Gather thermal conductivity cell detector 15 data by data processing stations 16, intuitively show finally by computer 17.
Described temperature programmed desorption test is: the second purge gas purges catalyst sample 13 at a set temperature through the second supply air line; After being down to 100 DEG C, switching six-way valve the 9, three reacting gas and pass into through the first supply air line that catalyst sample 13 is adsorbed is saturated; Again switch six-way valve 9, second purge gas again after the second supply air line passes into and purges catalyst sample 13 physisorption thing, the second side gas circuit through thermal conductivity cell detector 15 is emptying; Temperature programme makes catalyst sample 13 chemical absorption of surface species generation desorption, detects desorbed species signal with thermal conductivity cell detector 15; Gather thermal conductivity cell detector 15 data with data processing stations 16, intuitively show finally by computer 17.
The temperature programmed reduction test provided in this example, temperature programmed oxidation test and temperature programmed desorption method of testing are compared by instantiation and prior art means, and test result is suitable with effect; Specific embodiment is as follows:
1, temperature programmed reduction test
Accurately take 10-1000mg catalyst sample 13 and be packed into U-shaped reaction tube 10, thermopair 12 is inserted beds, installs heating furnace 11; High-purity N
2after deriving from the gas cylinder 1 of the first supply air line by reduction valve 3 controlled pressure within the scope of 0.1-0.5MPa, be 10-200ml/min through mass flowmeter 7 accurate flow control; High-purity N is controlled by switching six-way valve 9
2flow through beds along dotted line pipeline and carry out pre-service (purging) to make catalyst sample 13 clean surface to catalyst sample 13, pre-service (purging) condition is purge 0.5-1h at 100-500 DEG C.Meanwhile, 3%-10%H
2/ N
2(or CO/He) combination gas derive from the gas cylinder 2 of the second supply air line after by reduction valve 3 controlled pressure within the scope of 0.1-0.5MPa, be 10-100ml/min through mass flowmeter 7 accurate flow control; Emptying directly to be entered the second side gas circuit of thermal conductivity cell detector 15 after flowing through the first side gas circuit of thermal conductivity cell detector 15 along dotted line pipeline by six-way valve 9 after; Setting thermal conductivity cell detector 15 temperature is 60-120 DEG C, and bridge Current Control, within the scope of 50-100mA, starts image data and walks baseline.After catalyst sample 13 pre-service (purging), baseline is walked flat already, takes off the heating furnace 11 being in the condition of high temperature, changes the heating furnace 11 being in room temperature; Switch six-way valve 9 and make high-purity N
2directly emptying along solid line pipeline, 3%-10%H
2/ N
2(or CO/He) combination gas flows through beds along solid line pipeline, and in Temperature Programmed Processes, reduction reaction occurs for (heating rate is 5-20 DEG C/min) and catalyst sample 13, detects H by thermal conductivity cell detector 15
2(or CO) signal, finally records data by data processing stations 16 and display and preservation on computer 17.Other company's like product carries out the temperature programmed reduction test under same condition, and comparing result is if accompanying drawing 2 is (with 7%H
2/ N
2combination gas temperature programmed reduction CeO
2for example) shown in.Test result shows that the two test effect is suitable.
2, temperature programmed oxidation test
Temperature programmed oxidation test is on the basis of said procedure heating reduction, takes off the heating furnace 11 being in the condition of high temperature, changes the heating furnace 11 being in room temperature; Gas in second supply air line is switched to 2%-25%O
2/ N
2combination gas, by reduction valve 3 controlled pressure within the scope of 0.1-0.5MPa, is 10-100ml/min through mass flowmeter 7 accurate flow control; Beds is flowed through by six-way valve 9 along solid line pipeline after flowing through the first side gas circuit of thermal conductivity cell detector 15, the reducibility gas that the 0.5-1h that ventilates under room temperature remains with emptying, there is oxidation reaction in (heating rate is 5-20 DEG C/min) and the catalyst sample 13 after being reduced in Temperature Programmed Processes, detects O by thermal conductivity cell detector 15
2signal, finally records data by data processing stations 16 and display and preservation on computer 17.Other company's like product carries out the temperature programmed oxidation test under same condition, and comparing result is if accompanying drawing 3 is (with 20%O
2/ N
2the CuO/SiO that combination gas temperature programmed oxidation is reduced
2for example) shown in.Test result shows that the two test effect is suitable.
3, temperature programmed desorption test
Accurately take 50-1000mg catalyst sample 13 and be packed into U-shaped reaction tube 10, thermopair 12 is inserted beds, installs heating furnace 11; After high-purity He derives from the gas cylinder 2 of the second supply air line by reduction valve 3 controlled pressure within the scope of 0.1-0.5MPa, be 10-200ml/min through mass flowmeter 7 accurate flow control; Enter beds by six-way valve 9 along solid line pipeline after flowing through the first side gas circuit of thermal conductivity cell detector 15 and carry out pre-service (purging) to make catalyst sample 13 clean surface to catalyst sample 13, pre-service (purging) condition is purge 0.5-1h at 100-500 DEG C.After being down to 100 DEG C, 0.01%-2%NH
3/ He (or CO
2/ He or SO
2/ He or NO/He or O
2/ He) combination gas derive from the gas cylinder 1 of the first supply air line after by reduction valve 3 controlled pressure within the scope of 0.1-0.5MPa, be 10-100ml/min through mass flowmeter 7 accurate flow control; By switching six-way valve 9 control 0.01%-2%NH
3/ He (or CO
2/ He or SO
2/ He or NO/He or O
2/ He) combination gas flows through beds along dotted line pipeline makes catalyst sample 13 adsorb 0.5-2h until saturated at 100 DEG C.Then, enter beds by six-way valve 9 along solid line pipeline after switching six-way valve 9 makes high-purity He of 10-100ml/min flow through the first side gas circuit of thermal conductivity cell detector 15 to carry out purging 0.5-1h to remove the NH of physisorption to catalyst sample 13 at 100 DEG C
3(or CO
2or SO
2or NO or O
2), more emptying through the second side gas circuit of thermal conductivity cell detector 15.Meanwhile, setting thermal conductivity cell detector 15 temperature is 60-120 DEG C, and bridge Current Control, within the scope of 50-100mA, starts image data and walks baseline.Sweep after complete (baseline is walked flat already) until catalyst sample 13 physisorption air-blowing, heat up from 100 DEG C of start programs, the chemisorption species generation desorption on (heating rate is 5-20 DEG C/min) catalyst sample 13 surface in Temperature Programmed Processes, detect desorbed species signal by thermal conductivity cell detector 15, finally record data by data processing stations 16 and display and preservation on computer 17.Other company's like product carries out the temperature programmed desorption test under same condition, and comparing result such as accompanying drawing 4 (purges through 1%NH with high-purity He
3/ He combination gas adsorbs saturated CeO
2its generating program desorption by heating is made to be example) shown in.Test result shows that the two test effect is suitable.
The present invention can realize the switching of two-way gas easily, walks the object that baseline step can carry out simultaneously, greatly save the time, improve testing efficiency with what reach pre-service (purging) process of catalyst sample and instrument; Be equipped with 3 plug-in heating furnaces, facilitate the replacing of high-temperature heater, save the stand-by period of heating furnace cooling, improve testing efficiency, and test result is accurate.
Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (10)
1. a temperature programme analytical equipment, test for temperature programmed reduction, temperature programmed oxidation and temperature programmed desorption, it is characterized in that: comprise the first supply air line, the second supply air line, reactor, heating arrangement, thermal conductivity cell detector and six-way valve, described first supply air line is connected with the first interface of six-way valve, second supply air line is connected with the 3rd interface of six-way valve by after the first side gas circuit of thermal conductivity cell detector, emptying after the 4th interface of six-way valve connects the second side gas circuit of thermal conductivity cell detector by the road; Described reactor is arranged in heating arrangement, and the air intake opening of reactor and gas outlet are connected respectively by the second interface of pipeline and six-way valve and the 5th interface, and the 6th interface of described six-way valve is emptying.
2. temperature programme analytical equipment according to claim 1, it is characterized in that: described first supply air line and the second supply air line include the gas cylinder, reduction valve, pressure maintaining valve, permanent flow valve, tensimeter, mass flowmeter and the retaining valve that are successively set on gas circuit pipeline, the described retaining valve of the first supply air line is connected with the first interface of six-way valve, and the retaining valve of described second supply air line is connected with the first side gas circuit of thermal conductivity cell detector.
3. temperature programme analytical equipment according to claim 1, it is characterized in that: also comprise data processing stations and computer, described data processing stations is connected with thermal conductivity cell detector and computer respectively, carries out data processing and transmission.
4. temperature programme analytical equipment according to claim 1, is characterized in that: also comprise detector unit and temperature controller, the beds in described detector unit intercalation reaction device, and is connected with temperature controller, and described temperature controller is connected with heating arrangement.
5. temperature programme analytical equipment according to claim 4, is characterized in that: described detector unit is thermoelectricity occasionally temperature sensor.
6. temperature programme analytical equipment according to claim 1, is characterized in that: described reactor is U-shaped reaction tube, and described heating arrangement is plug-in type heating furnace, comprises a work heating furnace and at least one supplementary heater.
7. temperature programme analytical equipment according to claim 1, is characterized in that: the gas passed in described first supply air line is high-purity N
2, 0.01%-2%NH
3/ He combination gas, 0.01%-2%CO
2/ He combination gas, 0.01%-2%SO
2/ He combination gas, 0.01%-2%NO/He combination gas or 0.01%-2%O
2/ He combination gas; The gas passed in second supply air line is 3%-10%H
2/ N
2combination gas, 3%-10%CO/He combination gas, 2%-25%O
2/ N
2combination gas or high-purity He.
8. a property detection method for catalyzer, comprises temperature programmed reduction test, temperature programmed oxidation test and temperature programmed desorption test, also comprises the temperature programme analytical equipment described in claim 1 to 7 any one, it is characterized in that:
Described temperature programmed reduction test is: the first purge gas purges catalyst sample at a set temperature through the first supply air line; After being down to room temperature, switch six-way valve and make the first supply air line emptying through the 6th interface, the first reacting gas flows through beds through the second supply air line, and temperature programme makes the first reacting gas and catalyst sample generation reduction reaction; Then the first reacting gas signal is detected with thermal conductivity cell detector;
Described temperature programmed oxidation test is: after the reduction reaction of said procedure heating reduction test completes and is down to room temperature, first reacting gas is switched to the second reacting gas, and temperature programme makes the second reacting gas and the catalyst sample generation oxidation reaction be reduced; Then the second reacting gas signal is detected with thermal conductivity cell detector;
Described temperature programmed desorption test is: the second purge gas purges catalyst sample at a set temperature through the second supply air line; After being down to 100 DEG C, switch six-way valve, the 3rd reacting gas passes into through the first supply air line and makes catalyst sample absorption saturated; Again switch six-way valve, the second purge gas is again after the second supply air line passes into and purges catalyst sample physisorption thing, and the second side gas circuit through thermal conductivity cell detector is emptying; Temperature programme makes catalyst sample chemical absorption of surface species generation desorption, detects desorbed species signal with thermal conductivity cell detector;
Exported after above-mentioned thermal conductivity cell detector signal data is gathered by data processing stations.
9. the property detection method of catalyzer according to claim 8, it is characterized in that: in described temperature programmed reduction test, the walking baseline and can carry out simultaneously of the preprocessing process of catalyst sample and instrument: the first purge gas is when the first supply air line purges catalyst sample, entered the second side gas circuit of thermal conductivity cell detector after first reacting gas can flow through the first side gas circuit of thermal conductivity cell detector by six-way valve, thermal conductivity cell detector is normally worked, instrument normally walks baseline.
10. the property detection method of catalyzer according to claim 8, is characterized in that: described first purge gas is high-purity N
2, described first reacting gas is H
2/ N
2or CO/He combination gas, described second reacting gas is O
2/ N
2combination gas, described second purge gas is high-purity He, and described 3rd reacting gas is NH
3/ He combination gas, CO
2/ He combination gas, SO
2/ He combination gas, NO/He combination gas or O
2/ He combination gas.
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