CN102359989A - Multifunctional catalyst reaction evaluation and characterization device and application thereof - Google Patents

Multifunctional catalyst reaction evaluation and characterization device and application thereof Download PDF

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CN102359989A
CN102359989A CN2011102006348A CN201110200634A CN102359989A CN 102359989 A CN102359989 A CN 102359989A CN 2011102006348 A CN2011102006348 A CN 2011102006348A CN 201110200634 A CN201110200634 A CN 201110200634A CN 102359989 A CN102359989 A CN 102359989A
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gas circuit
gas
reaction
pipeline
way electromagnetic
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CN102359989B (en
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李永立
朱志荣
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SHANGHAI SHANGJIQUNLI ANALYTICAL INSTRUMENT CO Ltd
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SHANGHAI SHANGJIQUNLI ANALYTICAL INSTRUMENT CO Ltd
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Abstract

The invention provides a multifunctional catalyst reaction evaluation and characterization device and application thereof. The characterization device comprises a gas circuit control component, a catalytic reaction component, a detection function switching component, a signal detection processing component and a detection gas circuit balancing component. The multifunctional catalyst reaction evaluation and characterization device has the advantages that gas chromatography thermal conductivity detection, hydrogen flame ionization detection and catalyst evaluation systems are integrated, different detection modes are realized by different combination of electromagnetic valves, and more than ten chromatographic analysis and catalyst reaction evaluation and characterization functions are realized by the aid of a catalytic reaction portion.

Description

A kind of multifunction catalyst reaction evaluating characterization apparatus and application thereof
Technical field
The present invention relates to a kind of catalyst test apparatus, particularly relate to a kind of multifunction catalyst reaction evaluating characterization apparatus.
Background technology
The catalytic reaction technology played crucial effect in the chemical industry in modern age, the chemicals that uses in people's life at present all directly or indirectly relies on catalysis technique production and obtains more than 85%.Therefore, in Study of Catalyst and production run, the assay of catalyzer physicochemical property is most important, and it is the basis of understanding catalytic mechanism and design catalyzer, also is the means of control product quality in the Catalyst Production.Although along with the new catalyst characterization method of science and technology development constantly occurs, be most important link in the catalyst characterization in recent years always and come the way of assay catalysis material by gas chromatographic technique.
At present; Characterize aspect the catalyzer program of an additional cover temperature programme catalyst reaction device before the commodity gas phase analyzer often in chromatographic process, require further to add assembly (like six three-way electromagnetic valve door sampling apparatuses etc.) according to different signs and reach the purpose that corresponding catalyst analysis is estimated.At the online sampling analysis device of disclosed patent CN96211985.7, the quick on-line sampling sampling device of patent CN200610041677.5 multi-channel gas and catalyst performance evaluation system; And in these patent documentations of a patent CN200710064984.X miniature reactor-gas-chromatography combinatorial analysis evaluating system; Wherein gas chromatography is only as reaction product on-line analysis function; Save analysis time, improve accuracy, but can not carry out the mensuration sign of other performance of catalyzer.Simultaneously, this type apparatus function is often more single, and simultaneously catalytic reaction assembly and stratographic analysis assembly are separate, cause the bulky of equipment set, and the maintenance and the lab space utilization of instrument all brought many inconvenience.Purposes according to investigating existing simple type chromatogram characterization apparatus in many ways is confined at temperature programmed reduction (TPR); Temperature programmed desorption (TPD); Few functions aspects such as pulse catalytic reactor can't really satisfy chromatography and be used for the multifunction demand that the catalyst property multianalysis detects.
Therefore; We need a kind of device of evaluating catalyst; Can catalytic reaction and stratographic analysis be combined, and realize pulse and continuous catalytic reaction, the real-time sampling sample introduction analysis of catalytic reaction and the multiple functions such as physicochemical characteristics evaluation of catalyzer of catalyzer.
Summary of the invention
For solving the deficiency of prior art; First purpose of the present invention is; Provide a kind of catalyst reaction to estimate characterization apparatus; It is combined as a whole gas chromatographic analysis detection and catalyst reaction evaluation, Catalyst Characterization System, realizes that multiple stratographic analysis and catalyst reaction evaluation, catalyst property characterize function.
Second purpose of the present invention is, provides above-mentioned catalyst reaction to estimate the application of characterization apparatus.
For realizing first purpose, the technical scheme that the present invention takes is:
A kind of catalyst reaction is estimated characterization apparatus; Comprise: gas circuit Control Component, catalytic reaction assembly, measuring ability changeover module, input processing components and detection gas circuit balanced component; Said gas circuit Control Component, catalytic reaction assembly, measuring ability changeover module and detection gas circuit balanced component are connected through pipeline successively, and said input processing components is connected through pipeline with the measuring ability changeover module.
Said gas circuit Control Component comprises several air intake openings and solenoid valve.
Preferably, said gas circuit Control Component comprises four air intake openings and three four way solenoid valves, with said gas circuit Control Component be divided into three carrier gas with (or) the reaction gas gas circuit.
Preferably, said each carrier gas with (or) the reaction gas gas circuit is provided with a mass flowmeter.More preferably, one of them carrier gas with (or) the reaction gas gas circuit also is provided with a needle valve, said needle valve is located at before the mass flowmeter; All the other gas circuits come together in a three-way solenoid valve.
Said gas circuit Control Component be responsible for switching with the control catalyst assay in carrier gas and reactant gas; Switch the flow direction of carrier gas or reaction gas gas through said solenoid valve; Through the mass flowmeter of automatic control and the flow velocity of needle valve control carrier gas or reaction gas gas, wherein needle valve plays the effect of fine setting gas flow rate.
Said catalytic reaction assembly comprises the attemperating unit of reactor and this temperature of reactor of may command.
Preferably; Said catalytic reaction assembly also comprises one six three-way electromagnetic valve; Said six three-way electromagnetic valves are connected through pipeline with reactor successively; Said six three-way electromagnetic valves are connected through pipeline with the gas circuit Control Component, and said reactor is connected through pipeline with the measuring ability changeover module, and said attemperating unit is electrically connected with reactor.
More preferably; On the connecting tube of six three-way electromagnetic valves and gas circuit Control Component, on the connecting tube of reactor and measuring ability changeover module and six three-way electromagnetic valves and and reactor between connecting tube on; Be respectively equipped with and break off mouth, said disconnection mouth is used for optionally connecting different annexes.Said annex is selected from, but is not limited to, one or more in liquid nitrogen condensation device, the steam bubble device.
Said catalytic reaction assembly is responsible for reactant is offered reactor with the gas or the impulse form of continuous flow, implements the catalyst characterization analytic process of multiple other function simultaneously.In order to realize the purpose of the system of simplifying the operation, this part has used several kinds of different functions annexes, can add in different choice of location as required.The catalytic reaction control system of this device can be selected the mode of six three-way electromagnetic valve pulse sample introductions or successive reaction thing sample introduction, has adopted annex mode and six three-way electromagnetic valves to combine simultaneously, can select two kinds of input modes of reactant gas or liquid.
Said measuring ability changeover module comprises stratographic analysis post and several solenoid valves.
Preferably, said measuring ability changeover module is connected in sequence through pipeline by the one or six three-way electromagnetic valve, four way solenoid valve, the two or six three-way electromagnetic valve; Said chromatographic column is connected through pipeline with arbitrary said six three-way electromagnetic valves, and this six three-way electromagnetic valve also is connected through pipeline with the input processing components with the catalytic reaction assembly.
Said input processing components comprises a chromatogram detecting device and a signal processor.
Preferably, said chromatographic detector is thermal conductivity detector (TCD) (TCD detecting device) or flame ionization ditector (fid detector).
Said detection gas circuit balanced system contains several air intake openings.
Preferably, said detection gas circuit balanced system contains two air intake openings, is divided into 2 gas circuits, and each gas circuit is connected in sequence through pipeline by pressure maintaining valve, needle valve and injector.Arbitrary said gas circuit is connected through pipeline with the input processing components, and another gas circuit is connected through pipeline with the measuring ability changeover module.
The present invention also provides above-mentioned catalyst reaction to estimate the application of characterization apparatus in gas chromatographic analysis detection and catalyst reaction evaluation, catalyst characterization.Select different gas channels through switching solenoid valve, general formula adds different annexes, satisfies the different detection requirement.
The invention has the beneficial effects as follows: with the detection of gas chromatography thermal conductance, hydrogen flameionization detection and evaluating catalyst system combination is one; Various combination through solenoid valve is realized the different detection mode; In conjunction with catalytic reacting section, realize nearly stratographic analysis more than ten kinds and catalyst reaction evaluation and characterize function.
Description of drawings
Accompanying drawing 1 is a structural representation of the present invention;
Accompanying drawing 2 is that the present invention is used to measure TPR, TPD, the reaction wiring diagram of TPO and BET;
Accompanying drawing 3 is that the present invention carries out steam bubble continuous catalytic reaction process flow diagram;
Accompanying drawing 4 is that the present invention carries out steam pulse catalytic reactor process flow diagram.
Wherein:
1-gas circuit Control Component; 2-catalytic reaction assembly;
3-measuring ability changeover module; 4-input processing components;
5-detection gas circuit balanced component; 14-mass flowmeter;
22-reactor; The attemperating unit of 23-reactor;
33-chromatographic column; 41-signal amplifier;
42-signal output apparatus; 43-chromatographic detector.
Embodiment
For making above-mentioned purpose of the present invention, characteristic and advantage more obviously understandable, hereinafter is special lifts preferred embodiment of the present invention, and conjunction with figs., elaborates as follows.Moreover, the direction term that the present invention mentioned, for example " on ", D score, " preceding ", " back ", " left side ", " right side ", " interior ", " outward ", " side " etc., only be direction with reference to annexed drawings.Therefore, the direction term of use is in order to explanation and understands the present invention, but not in order to restriction the present invention.
See also accompanying drawing 1, a kind of catalyst reaction of the present invention is estimated characterization apparatus, comprising: gas circuit Control Component 1, catalytic reaction assembly 2, measuring ability changeover module 3, input processing components 4 and detection gas circuit balanced component 5.
Said gas circuit Control Component 1 comprises 4 air intake openings and 3 four way solenoid valves 11, with said gas circuit Control Component 1 be divided into 3 carrier gas with (or) the reaction gas gas circuit (and a, b, c).Each carrier gas with (or) (a, b c) are provided with a mass flowmeter 14 to the reaction gas gas circuit.
Please continue referring to accompanying drawing 1, carrier gas with (or) also be provided with a needle valve 13 on the reaction gas gas circuit c, said needle valve 13 is located at before the mass flowmeter 14; Gas circuit a and b come together in three-way solenoid valve 12.Through using four way solenoid valve 11 and three-way solenoid valve 12 to realize switching the flow direction of carrier gas and reaction gas, realize controlling the flow velocity of carrier gas and reaction gas through mass flowmeter 14 and the needle valve 13 that uses automatic control, said needle valve 13 is used to finely tune gas flow rate.
Please continue to consult accompanying drawing 1, said catalytic reaction assembly 2 comprises the attemperating unit 23 of six three-way electromagnetic valves 21, reactor 22 and controlling reactor 22 temperature.The left side of said six three-way electromagnetic valves 21 is connected through pipeline with c road gas circuit with the three-way solenoid valve 12 of gas circuit Control Component 1 respectively, and the right side of six three-way electromagnetic valves 21 links to each other with reactor 22.Said six three-way electromagnetic valves 21 are equipped with the disconnection mouth with c road gas circuit connecting place, six three-way electromagnetic valves 21 of gas circuit Control Component 1 with the junction of sample introduction reactor 22 and the junction of reactor 22 and measuring ability changeover module; Be among Fig. 1, the right side of the left and right sides of six three-way electromagnetic valves 21 and reactor 22 is equipped with breaks off mouth.Said disconnection mouth is used to connect different annexes, like steam bubble device and the condenser in the accompanying drawing 1.Also be connected with volumetric bottle 24 on said six three-way electromagnetic valves 21, be used to realize the impulse form sample introduction.
Like this, the present invention can offer reactor 22 with the gas or the impulse form of continuous flow with reactant, realizes two kinds of input modes of six three-way electromagnetic valve pulses and successive reaction thing.Simultaneously, through add several kinds of different annexes in different choice of location, can implement the catalyst characterization analytic process of multiple other function.Adopt annex mode and six three-way electromagnetic valves to combine simultaneously, can select two kinds of input modes of reactant gas or liquid.
Please continue to consult accompanying drawing 1, said measuring ability changeover module 3 is connected in sequence through pipeline by the one or six three-way electromagnetic valve 31, four way solenoid valve 32 and the two or six three-way electromagnetic valve 34.Wherein the reactor 22 in the two or six three-way electromagnetic valve 34 and chromatographic column 33, the catalytic reaction assembly links to each other with chromatographic detector 43 in the input processing components; The one or six three-way electromagnetic valve 31 is connected with gas circuit e in detecting gas circuit balanced system 5.Said the one or six three-way electromagnetic valve 31 also is connected with certain measuring bottle 35, is used to realize the pulse sample introduction.
Through utilizing the various combination of six three-way electromagnetic valves 31,34 and four way solenoid valve 32; Can select to generate three kinds of diverse detection modes; That is: the successive reaction air-flow directly detects (as shown in Figure 2); The pulse reaction potpourri directly carries out detecting (as shown in Figure 4) after the chromatographic resolution, and successive reaction potpourri Pulse Chromatographic post separates back check and analysis (as shown in Figure 3).Just because of the multiple input mode of catalytic reaction assembly 2 and the use of annex; The different detection modes that combine measuring ability changeover module 3 simultaneously make the present invention realize pulse and continuous catalytic reaction, the real-time sampling sample introduction analysis of catalytic reaction and the multiple functions such as physicochemical characteristics evaluation of catalyzer of catalyzer simultaneously.
Please continue to consult accompanying drawing 1, said input processing components 4 comprises chromatographic detector 43 and signal processor, and said signal processor comprises signal amplifier 41 and signal output apparatus 42.Preferably, said chromatographic detector 43 is thermal conductivity detector (TCD) (TCD).
The collection that said input processing components 4 is responsible for detection signal is amplified and output.
Please continue to consult accompanying drawing 1, said detection gas circuit balanced system 5 contains 2 air intake openings, is divided into 2 tunnel gas circuits (d, e), and each gas circuit (d, e) is respectively by pressure maintaining valve 51, and needle valve 52 and injector 53 are connected in sequence through pipeline.Gas circuit d is connected with chromatographic detector 43 in the input processing components 4.
Required balanced gas or carrier gas in the said detection gas circuit balanced system 5 control detection function changeover modules.
During use, the gas circuit d and the e of open detection gas circuit balanced system 5 add H 2Or He gas, six three-way electromagnetic valves 31 and 34 in the change detection function switched system 3, the temperature control of opening chromatographic column, input disposal system and each assembly can realize stratographic analysis.
Accompanying drawing 2 is that apparatus of the present invention are used for temperature programmed reduction reaction (TPR), temperature programmed desorption (TPD), and the reaction wiring diagram of temperature programmed oxidation reaction (TPO) and specific area measuring (BET), dotted line is a conducting state among the figure, solid line is a closure state.
See also accompanying drawing 2, open the gas circuit d that detects gas circuit balanced system 5 and be written into He gas, open gas circuit a and b in the gas circuit Control Component 1, and in gas circuit a, be written into reaction gas H 2, O 2Or N 2, in gas circuit b, be written into He gas.Like this, be carrier gas with He, mix H simultaneously 2, can carry out temperature programmed reduction reaction (TPR); With He is carrier gas, mixes O simultaneously 2, can carry out temperature programmed oxidation reaction (TPO); With He is carrier gas, mixes N simultaneously 2Gas can be measured the specific surface area (BET) of catalyzer.Under the condition of measurement the specific area, use condenser as annex; In the process of temperature programmed surface reaction, select the chromatographic column in the measuring ability changeover module 3 to separate simultaneously, and with six logical mode sample introductions, composition that can the on-line analysis reaction product.
See also accompanying drawing 3, accompanying drawing 3 is that the present invention carries out steam bubble continuous catalytic reaction process flow diagram.Only open the gas circuit b in the gas circuit Control Component 1 and be written into H 2, the gap between six three-way electromagnetic valves 21 and sample introduction reactor 22 connects the steam bubble device.Like this, make H 2Through the bubbling mode, liquid reactants is taken in the reactor 32, after the continuous catalytic hydrogenation reaction, get into measuring ability changeover module 3.With after chromatographic column 33 is separated, entering chromatographic detector 43 carries out stratographic analysis through the sampling of six three-way electromagnetic valves 31.
This flow process also can be carried out oxidation reaction, the reaction of other type such as isomerization reaction except hydrogenation reaction.
See also accompanying drawing 4, accompanying drawing 4 is that the present invention carries out steam pulse catalytic reactor process flow diagram.Open gas circuit b and c in the gas circuit Control Component 1, be written into H respectively 2And N 2Be connected the steam bubble device at six three-way electromagnetic valves 21 with the disconnection mouth of gas circuit c junction.Through using N 2Or H 2The bubbling organic liquid utilizes quantity tube 24 sample introductions of six three-way electromagnetic valves 21, with H 2As reaction gas, carry out hydrogenation reaction.Then, through the gas after the hydrogenation reaction in measuring ability changeover module 3, after separating through chromatographic column 33, entering signal detecting processing system output-response result.
This reaction can be selected cracking reaction, isomerization reaction etc. simultaneously.
In all flow processs, can carry out the pre-service under the differential responses condition according to the requirement of catalyzer.
Several concrete testing processes below are provided.
Embodiment 1
The TPD function characterizes acidity of catalyst matter: place catalyst reaction to estimate the reaction tube of characterization apparatus in 0.205g 40~60 purpose ZSM-5 molecular sieve catalyst samples, and reaction tube is put into reactor 22.TPR/TPD/ TPO and BET that device is switched to like accompanying drawing 2 measure the path mode.In gas circuit b, feed helium, through temperature in the attemperating unit 23 conditioned reaction devices 22 as for 550 ℃.(helium flow velocity 25 ml/min) 550 ℃ carry out pre-service 2 h to sample under helium atmosphere, are cooled to 120 ℃ then.Stop helium and supply with, and in gas circuit a, feed ammonia, through the situation of the said catalyzer absorbing ammonia of signal output apparatus 42 observations.When signal output apparatus 42 shows the catalyzer absorbing ammonia to saturation balance, close gas circuit a and supply with, and open gas circuit b to stop ammonia, use the helium purge sample.After treating that detection signal baseline that signal output apparatus 42 shows is walked steadily; The temperature programmed desorption of beginning sample introduction reactor 22; Temperature rises to 650 ℃ from 120 ℃ of heating rates with 10 ℃/min, on signal output apparatus 42, obtains the ammonia signal curve of continuous detecting desorption, and the temperature section of pressing the desorption ammonia is (than weak component I=120-330 ℃; Strong assembly II=330-550 ℃) quantitative Analysis goes out ammonia quantity (unit is: mM mmol); Be the surface acid amount of catalyzer, be respectively, strong assembly 0.310 mmol/g than weak component 0.652 mmol/g.
Embodiment 2
The TPR function characterizes catalyst reduction character: 0.212g 40~60 purpose alumina load nickel oxide catalyst samples are placed reaction tube, and reaction tube is put into reactor 22.TPR/TPD/ TPO and BET that device is switched to like accompanying drawing 2 measure the path mode.In gas circuit b, feed helium, through temperature in the attemperating unit 23 conditioned reaction devices 22 as for 550 ℃.(helium flow velocity 25 ml/min) 550 ℃ carry out pre-service 2 h to sample under helium atmosphere, are cooled to 120 ℃ then.Stop helium and supply with, and in gas circuit a, feed the argon gas that contains 20.0 % (wt) hydrogen, observe the situation of said catalyzer absorption argon gas through signal output apparatus 42.When signal output apparatus 42 shows that catalyzer absorption argon gas is to saturation balance; After the detection signal baseline of signal output apparatus 42 was steady, the temperature programme of beginning reactor 22 characterized, and temperature rises to 700 ℃ from 120 ℃ of heating rates with 10 ℃/min; Oxide reduction consumption hydrogen formed signal curve during continuous detecting heated up; Observe 330 ℃ and 550 ℃ of two reduction peak, explain that the load nickel oxide catalyst is reduced to nickel step by step, but quantitative Analysis goes out to consume H simultaneously 2(unit is quantity: mM mmol), be surface nickel amount 0.346 mmol/g (being nickeliferous 2.0 % (wt)) of catalyzer.
Embodiment 3
The TPO function characterizes catalyst reduction character: use the Y molecular sieve catalyzer 0.238g sample of coking (carbon distribution) to place reaction tube the reaction of 40~60 purposes, and reaction tube is put into reactor 22.TPR/TPD/ TPO and BET that device is switched to like accompanying drawing 2 measure the path mode.In gas circuit b, feed helium, through temperature in the attemperating unit 23 conditioned reaction devices 22 as for 400 ℃.(helium flow velocity 25 ml/min) 400 ℃ carry out pre-service 2 h to sample under helium atmosphere, are cooled to 120 ℃ then.Stop helium and supply with, and in gas circuit a, feed the argon gas that contains 10.0 % (wt) oxygen, observe the situation of said catalyzer absorption argon gas through signal output apparatus 42.When signal output apparatus 42 shows that catalyzer absorption argon gas is to saturation balance; After the detection signal baseline that signal output apparatus 42 shows is walked steadily; The temperature programme of beginning sample introduction reactor 22 characterizes; Temperature rises to 800 ℃ from 120 ℃ of heating rates with 10 ℃/min, coking oxidation consumption O during continuous detecting heats up 2Form signal curve, observe, explain that the coking of Y molecular sieve catalyzer is oxidized to CO step by step 330 ℃ and 550 ℃ of two oxidation peak 2But quantitative Analysis goes out to consume O simultaneously 2(unit is quantity: mM mmol), be surface carbon amount 0.713 mmol/g (being carbon distribution 0.86 % (wt)) of catalyzer.
Embodiment 4
The BET function characterizes catalyst surface area: the MOR molecular sieve catalyst 0.361g sample more than 100 orders is placed the cold-trap pipe, and TPR/TPD/ TPO and BET that device is switched to like accompanying drawing 2 measure the path mode.In gas circuit b, feed helium, (helium flow velocity 25 ml/min) 500 ℃ of pre-service 2 h are cooled to room temperature then under helium atmosphere; The cold-trap pipe is immersed in the liquid nitrogen cup, feed the helium that contains 5.0 % (V/V) nitrogen, be adsorbed to saturation balance; After signal base line to be detected is walked steadily; The liquid nitrogen cup is changed into greater than 90 ℃ of hot water cups, and desorption discharged nitrogen and forms signal curve during continuous detecting heated up, but quantitative Analysis goes out desorption nitrogen quantity (mM mmol) simultaneously; Repeat above-mentioned adsorption-desorption process, measure desorption N under the helium that contains 10.0 % (wt), 20.0% (V/V) nitrogen respectively 2The surface area that quantity, Application of B ET formula calculate catalyzer is 329 m 2/ g.
Embodiment 5
The continuous catalysis of catalyzer (isopropyl benzene cracking) reaction evaluating: the ZSM-5 molecular sieve catalyst sample more than 0.520g 40~60 orders is placed reaction tube, and reaction tube is put into reactor 22.Device is switched to the steam bubble continuous catalytic reaction path mode of Fig. 3.(helium flow velocity 25 ml/min) 450 ℃ carry out pre-service 2 h to sample under helium atmosphere; Be cooled to 390 ℃ of temperature of reaction then; Isopropyl benzene is packed in the steam bubble pipe, immerse in 80 ℃ of hot water cups, feed the helium of 25 ml/min and react through sample introduction reactor 22.After 30 minutes, switch the two or six three-way electromagnetic valve 34; Negate answers the product gas sample to carry out stratographic analysis; Detect the content of isopropyl benzene and benzene; Quantitative Analysis goes out isopropyl benzene conversion ratio and benzene yield, records the isopropyl benzene conversion ratio 84.7% (wt) and benzene yield 93.1 % (wt) of catalyzer respectively, explains that catalyzer has than high reaction activity and selectivity.
Embodiment 6
The continuous catalysis of catalyzer (xylene isomerization) reaction evaluating: the supporting Pt more than 0.415g 40~60 orders/ZSM-5 molecular sieve catalyst sample is placed reaction tube, and device is switched to the steam pulse catalytic reactor path mode shown in accompanying drawing 4.In gas circuit b, feed hydrogen, (flow velocity 25 ml/min) 460 ℃ of pre-service 2 h are cooled to 400 ℃ of temperature of reaction then under hydrogen atmosphere; With m-xylene with in the steam bubble pipe of packing into; Immerse in 80 ℃ of hot water cups, the hydrogen that feeds 25 ml/min is every after 30 minutes, switches six three-way electromagnetic valves 21; Through quantity tube 24 intercepting reactants (quantity tube is 100 microlitres); Feed sample introduction reactor 22 and react, product gas sample on-line chromatograph is analyzed, and detects the content of o-xylene, P-xylene and m-xylene; It is 46.1% (wt) and o-xylene yield 93.1% (wt), P-xylene yield that quantitative Analysis goes out the m-xylene conversion ratio, explains that catalyzer has higher reaction conversion ratio and selectivity of product.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the present invention's design; Can also make some changes, improvement and retouching, these changes, improvement and retouching also should be regarded as protection scope of the present invention.

Claims (10)

1. multifunction catalyst reaction evaluating characterization apparatus is characterized in that said characterization apparatus comprises:
-gas circuit Control Component comprises several air intake openings and solenoid valve;
-catalytic reaction assembly comprises the attemperating unit of reactor and this temperature of reactor of may command;
-measuring ability changeover module comprises stratographic analysis post and several solenoid valves;
-input processing components comprises chromatographic detector and signal processor;
-detect the gas circuit balanced component, comprise several air intake openings;
Said gas circuit Control Component, catalytic reaction assembly, measuring ability changeover module and detection gas circuit balanced component are connected through pipeline successively, and said input processing components is connected through pipeline with the measuring ability changeover module.
2. catalyst reaction according to claim 1 is estimated characterization apparatus; It is characterized in that; Said catalytic reaction assembly also comprises one six three-way electromagnetic valve, and said six three-way electromagnetic valves are connected through pipeline with reactor successively, and said six three-way electromagnetic valves are connected through pipeline with the gas circuit Control Component; Said reactor is connected through pipeline with the measuring ability changeover module, and said attemperating unit is electrically connected with reactor.
3. catalyst reaction according to claim 2 is estimated characterization apparatus; It is characterized in that; On the connecting tube of six three-way electromagnetic valves and gas circuit Control Component, on the connecting tube of reactor and measuring ability changeover module and six three-way electromagnetic valves and and reactor between connecting tube on; Be respectively equipped with and break off mouth, said disconnection mouth is used for optionally connecting different annexes.
4. catalyst reaction according to claim 1 is estimated characterization apparatus, it is characterized in that said measuring ability changeover module is connected in sequence through pipeline by the one or six three-way electromagnetic valve, four way solenoid valve, the two or six three-way electromagnetic valve; Said chromatographic column is connected through pipeline with arbitrary said six three-way electromagnetic valves, and this six three-way electromagnetic valve also is connected through pipeline with the input processing components with the catalytic reaction assembly.
5. catalyst reaction according to claim 1 is estimated characterization apparatus, it is characterized in that said chromatographic detector is thermal conductivity detector (TCD) or flame ionization ditector.
6. catalyst reaction according to claim 1 is estimated characterization apparatus, it is characterized in that said detection gas circuit balanced system contains two air intake openings, is divided into two gas circuits, and each gas circuit is connected in sequence through pipeline by pressure maintaining valve, needle valve and injector; Wherein arbitrary said gas circuit is connected through pipeline with the input processing components, and another gas circuit is connected through pipeline with the measuring ability changeover module.
7. estimate characterization apparatus according to the arbitrary described catalyst reaction of claim 1-6, it is characterized in that said gas circuit Control Component comprises four air intake openings and three four way solenoid valves, with said gas circuit Control Component be divided into three carrier gas with (or) the reaction gas gas circuit.
8. catalyst reaction according to claim 7 is estimated characterization apparatus, it is characterized in that, said each carrier gas with (or) the reaction gas gas circuit is provided with a mass flowmeter.
9. catalyst reaction according to claim 8 is estimated characterization apparatus, it is characterized in that, one of them carrier gas with (or) the reaction gas gas circuit also is provided with a needle valve, all the other gas circuits come together in a three-way solenoid valve.
10. the arbitrary described catalyst reaction of a claim 1-9 is estimated the application of characterization apparatus in gas chromatographic analysis detection and catalyst reaction evaluation, catalyst characterization.
CN 201110200634 2011-07-18 2011-07-18 Multifunctional catalyst reaction evaluation and characterization device and application thereof Expired - Fee Related CN102359989B (en)

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CN103558301B (en) * 2013-09-30 2015-05-13 华东师范大学 Micro-size catalyst in-situ pulse evaluation and analysis device
CN104062370B (en) * 2014-06-19 2016-01-20 中国天辰工程有限公司 A kind of take mixed gas as the gas chromatography method for quick of carrier gas

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1490620A (en) * 2003-08-26 2004-04-21 上海师范大学 Catalyst surface-characteristic comprehensive measuring device and application thereof
CN101776650A (en) * 2009-12-25 2010-07-14 昆明理工大学 Automatic gas-liquid-solid three phase catalytic reaction evaluation system
KR100993504B1 (en) * 2009-10-06 2010-11-10 (주)원익머트리얼즈 Analysis equipment for nitrogen monoxide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1490620A (en) * 2003-08-26 2004-04-21 上海师范大学 Catalyst surface-characteristic comprehensive measuring device and application thereof
KR100993504B1 (en) * 2009-10-06 2010-11-10 (주)원익머트리얼즈 Analysis equipment for nitrogen monoxide
CN101776650A (en) * 2009-12-25 2010-07-14 昆明理工大学 Automatic gas-liquid-solid three phase catalytic reaction evaluation system

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9844361B2 (en) 2012-05-29 2017-12-19 Koninklijke Philips N.V. Pulmonary ultrasound techniques for elastography in lungs
CN103901131B (en) * 2014-04-10 2015-04-15 中国科学院福建物质结构研究所 Device and method device for evaluating catalyst during preparation of oxalate through three-channel automatic CO gas phase oxidative coupling
CN103901131A (en) * 2014-04-10 2014-07-02 中国科学院福建物质结构研究所 Device and method device for evaluating catalyst during preparation of oxalate through three-channel automatic CO gas phase oxidative coupling
CN105445416A (en) * 2014-09-03 2016-03-30 湖南华思仪器有限公司 Dynamic adsorption instrument
CN105067752A (en) * 2015-07-24 2015-11-18 中国科学院重庆绿色智能技术研究院 Program heating analysis equipment and method for testing property of its catalyst
CN106802262B (en) * 2017-01-26 2019-05-28 王宏铭 A method of catalyst performance is tested using thermogravimetry
CN106802262A (en) * 2017-01-26 2017-06-06 芜湖市纽泰知识产权信息咨询有限公司 A kind of method that utilization DTG tests catalyst performance
CN107941986A (en) * 2017-10-19 2018-04-20 浙江大学 A kind of device for being used to evaluate catalyst catalytic performance
CN107941986B (en) * 2017-10-19 2020-05-29 浙江大学 Device for evaluating catalytic performance of catalyst
CN107884306A (en) * 2017-11-10 2018-04-06 郑州大学 A kind of adsorption test method and device
CN108426975A (en) * 2018-05-15 2018-08-21 东莞诺维新材料科技有限公司 A kind of catalyst activity evaluating apparatus
CN108426975B (en) * 2018-05-15 2023-12-26 东莞诺维新材料科技有限公司 Catalyst activity evaluation device
CN110220941A (en) * 2019-06-04 2019-09-10 江南大学 A kind of method of carbon distribution content inside and outside measurement micro porous molecular sieve
CN110907559A (en) * 2019-12-13 2020-03-24 武汉纺织大学 Universal fixed bed catalyst evaluation device
CN110907559B (en) * 2019-12-13 2022-04-08 武汉纺织大学 Universal fixed bed catalyst evaluation device

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