CN109541009A - A wire mesh rapid heating and fast mass spectrometry gas-solid phase analyzer - Google Patents
A wire mesh rapid heating and fast mass spectrometry gas-solid phase analyzer Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 150
- 239000007790 solid phase Substances 0.000 title abstract description 3
- 238000004949 mass spectrometry Methods 0.000 title abstract 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 106
- 238000012544 monitoring process Methods 0.000 claims abstract description 28
- 239000000376 reactant Substances 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims description 56
- 238000001819 mass spectrum Methods 0.000 claims description 54
- 238000004458 analytical method Methods 0.000 claims description 35
- 239000000523 sample Substances 0.000 claims description 34
- 239000007787 solid Substances 0.000 claims description 31
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- 239000007795 chemical reaction product Substances 0.000 abstract description 10
- 238000009792 diffusion process Methods 0.000 abstract description 8
- 238000007086 side reaction Methods 0.000 abstract description 3
- 238000009529 body temperature measurement Methods 0.000 abstract 2
- 239000010419 fine particle Substances 0.000 abstract 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 55
- 229910000019 calcium carbonate Inorganic materials 0.000 description 28
- 238000000354 decomposition reaction Methods 0.000 description 18
- 238000000034 method Methods 0.000 description 17
- 238000003746 solid phase reaction Methods 0.000 description 15
- 230000008569 process Effects 0.000 description 13
- 239000008187 granular material Substances 0.000 description 12
- 239000012159 carrier gas Substances 0.000 description 11
- 238000011160 research Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000012495 reaction gas Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 230000007246 mechanism Effects 0.000 description 7
- 230000004044 response Effects 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 238000007789 sealing Methods 0.000 description 5
- 239000002028 Biomass Substances 0.000 description 4
- 244000166124 Eucalyptus globulus Species 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000004088 simulation Methods 0.000 description 4
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- LIXXICXIKUPJBX-UHFFFAOYSA-N [Pt].[Rh].[Pt] Chemical compound [Pt].[Rh].[Pt] LIXXICXIKUPJBX-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
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- 238000005243 fluidization Methods 0.000 description 1
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- 238000002309 gasification Methods 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/622—Ion mobility spectrometry
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- Electrochemistry (AREA)
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- Spectroscopy & Molecular Physics (AREA)
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Abstract
本发明公开一种丝网急速加热和快速质谱气固相分析仪，包括急速加热单元、快速质谱在线监测系统、测温系统和电控系统。微细颗粒反应物放置在急速加热单元内进行急速升温反应，在反应的同时，通过气体输送与快速质谱在线监测系统获得实时的气体产物组成成分与浓度数据，通过测温系统获得准确实时的温度数据，急速加热单元在电控系统的设定调控下可达到的高达1000℃/s升温速率和1000℃加热最终温度。实现了对反应物在急速加热反应过程中产物组分的瞬时释放温度、释放量和产物组分浓度等反应信息的高速捕捉，为本征反应动力学研究提供数据基础。同时有效减少反应产物的逗留时间，降低副反应，抑制扩散影响，使得反应测试更接近化学反应的本征特征。
The invention discloses a wire mesh rapid heating and rapid mass spectrometry gas-solid phase analyzer, comprising a rapid heating unit, a rapid mass spectrometry online monitoring system, a temperature measurement system and an electric control system. The fine particle reactant is placed in the rapid heating unit for rapid heating reaction. At the same time of the reaction, real-time gas product composition and concentration data are obtained through the gas delivery and rapid mass spectrometry online monitoring system, and accurate real-time temperature data is obtained through the temperature measurement system. , the rapid heating unit can reach a heating rate of up to 1000°C/s and a final temperature of 1000°C under the setting and regulation of the electronic control system. The high-speed capture of reaction information such as the instantaneous release temperature, release amount, and product component concentration of the product components during the rapid heating reaction of the reactants is realized, which provides a data basis for the study of intrinsic reaction kinetics. At the same time, it effectively reduces the residence time of reaction products, reduces side reactions, and inhibits the influence of diffusion, so that the reaction test is closer to the intrinsic characteristics of chemical reactions.
Description
Technical field
The invention belongs to measuring instrument field, be related to be applied to Chemical Manufacture, using energy source, material preparation, thermal power generation,
The rapidly transient prediction gas-solid phase reaction in the industrial trades such as ore smelting field is analyzed.
Background technique
Gas-solid phase reaction analyzer is the important scientific research apparatus in the fields such as derived energy chemical, and many important industrial process relate to
And the fields such as gas-solid phase reaction, such as Chemical Manufacture, using energy source, material preparation, thermal power generation, ore smelting, typical gas
Solid phase reaction includes that the pyrolysis of biomass or coal, gasification, burning, the reducing/regenerating of catalyst, dry desulfurization consolidate sulphur etc..Gas-solid phase
Reaction normally comprises the processes such as heat transfer, convection current and diffusion, the absorption on the surface of solids and desorption, chemical reaction, has non-equal
The features such as phase, unstable state, numerous influence factor is an extremely complex process, therefore studies gas-solid phase reaction analysis test
Method has a very important significance many industrial process, has boundless application prospect and value.
The measurement of response characteristic and kinetics is starting point and the basis of gas-solid phase reaction science and technology and technological development,
Kinetics can reveal that the objective law that reaction process is followed, thus the optimization of the design and processes condition for heater
Theoretical foundation is provided.
The research method of gas-solid reaction kinetic includes experimental analysis test and acquisition reaction kinetics equation two at present
Step, wherein experimental data is to obtain the basis of kinetics equation, and the degree of closeness with real reaction process is to obtained
The order of accuarcy of reaction Kinetics Model has vital influence.Currently used gas-solid phase reaction test method is in addition to certainly
Outside the various microminiature heaters of row design, there are also heat analysis, microscopic analysis, diffraction analysis, wave spectrum, spectrum and electricity, magnetic survey
The methods of amount, wherein heat analysis because its amount of samples is few, experimental period is short, convenient for quantifying reaction rate and accurately control temperature etc.
Advantage becomes current main stream approach, and thermogravimetric analyzer is most commonly used a kind of instrument in heat analysis application, and this method is
The quality of sample is measured under programed temperature with the variation relation of temperature (or time), but is limited to existing thermogravimetric analysis
The structure and principle of instrument, on the one hand maximum heating rate is relatively slow (only 1.67 DEG C/s), and temperature lag is serious, with up to 500-
The practical gas-solid reaction rate of 1000 DEG C/s differs greatly, therefore its reactive kinetics parameters for measuring and real reaction not phase
Symbol；On the other hand, the test process of diffusion couple thermogravimetric analysis influences great, offsets from intrinsic reaction process；Therefore it tested
Cheng Buneng really analyzes test real reaction, and there are biggish deviations for result and the real process rapidly to heat up reaction, sternly
Ghost image rings the research of reaction mechanism.The temperature programming of thermogravimetric simultaneously deviates setting value vulnerable to system heat absorption/exothermic influence, because
The experimental technique and analysis instrument of the new new gas-solid phase reaction of this exploitation using obtain accurately and reliably experimental data as analyzing
It is most important to the further further investigation for pushing gas-solid phase reaction analysis to calculate basis.
Based on the above problem existing for thermogravimetric analyzer, current many researchers devise a variety of heaters to study it
Specific reactive kinetics parameters.Such as Naruse develops a kind of heating furnace that can move up and down.The furnace is first by atmosphere
Gas be heated to specific temperature, it is then that the reaction member equipped with reaction mass is chemical anti-by quickly moving up and starting
It answers.Furthermore the fast decoupled characteristic of fuel is also used to by the variation of the gaseous products after analysis reaction, but these are heated
Device usually all has biggish size, and the processes such as gas mixing, diffusion existing for these heaters must draw during the experiment
The significant errors for playing measurement data, influence the reliability and reproducibility of institute's test reaction dynamics data.Especially as biomass
Such fast reaction process is decomposed, the correct measurement of reaction speed is that these heaters cannot achieve.Simultaneously because these
Heater be mostly make by oneself, test result will be different with the difference of the parameter of heater, cause experimental data it is very scattered,
System, difference is not big.
Based on the product analysis for reproducing transient response, therefore light text etc. develops a kind of miniature fluidized bed isothermal differential perhaps
(gas) solid phase reaction analyzer, the analyzer using miniature fluidized bed be used as heater, integrate solid material transient pulse with
Gaseous product on-line monitoring, realizes low diffusion isothermal differential response characteristic, but due to its fluidization characteristic, which can not be treated
The temperature-rise period for surveying particle measures, and cannot achieve and reaction temperature and reactant composition and its characteristic are mapped, therefore
There are still insufficient and defects for accurate research dynamic (dynamical) to gas-solid phase reaction.In order to accurately carry out grinding for gas-solid phase reaction mechanism
Study carefully, establish accurate prediction model, it is necessary to obtain the reaction rate that the rate of heat addition in temperature-rise period is up to 102-105 DEG C/s.But
Due to the interaction between heat transfer, mass transfer and chemical reaction, in particular with grain shape in heat transfer reaction process, thermal capacitance,
The thermophysical properties such as emissivity and thermal conductivity and change so that Accurate Prediction is more difficult.
From research both at home and abroad above as can be seen that research and development energy accurate simulation reaction process (especially overcomes and extends influence, rises
Warm process is faster), adaptability is wider, professional stronger gas-solid reaction kinetic analysis instrument has important practical significance and
Scientific meaning.The present invention exactly proposes that the instrument has heating speed compared with traditional thermogravimetric analyzer in view of the above problems
Rate fast (500-1000 DEG C/s), extend influence the advantages that low, performance is stable, control precision is high, provides for the research of reaction mechanism
More accurate means all have stronger novelty in thinking and technology.
Patent of invention content
In order to overcome the above-mentioned deficiencies of the prior art, the present invention proposes a kind of silk screen instant heating and quick mass spectrum gas-solid
Facies analysis instrument, it is core, the quick matter of integrated gas product constituent and concentration which, which is using silk screen flash heater,
On-line monitoring system is composed, it can be anti-to subparticle reactant progress quantitative sample injection, instant heating, minimal diffusion inhibition, differentiation
It should be captured with Millisecond reaction information, realize the instantaneous relase temperature to reactant product component during rapidly temperature reaction
Degree, instantaneous relase amount and the on-line monitoring for organizing sub-sequence.
In order to achieve the above object, the invention proposes technical solutions below:
A kind of silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument, including instant heating unit, quick mass spectrum are online
Monitoring system, temp measuring system and electric-control system, the instant heating unit are supervised by special purpose interface with the quick mass spectrum online
Examining system seamless connection, subparticle reactant, which is placed in the instant heating unit, carries out rapidly temperature reaction, the urgency
Fast heating unit realizes the requirement of different heating rates and different heating final temperatures under the control of the electric-control system, by described
Quick mass spectrum on-line monitoring system can get reaction product component and concentration data, be obtained by the temp measuring system anti-in real time
Answer object heating data.
The instant heating unit includes the heater body and heater upper cover for placing subparticle reactant, institute
The two sides for stating heater body upper end are respectively arranged with electrode, and the electrode of two sides is equipped with lower layer's heating net, on the heater
It is covered with upper layer heating net and pressing device, the upper layer heating net and lower layer's heating net are pressed in described by the pressing device
Electrode, the electrode are connect by conducting wire with the electric-control system.
The special purpose interface includes capillary sample feeding pipe, heating tube, the insulating tube set gradually from the inside to the outside, in the capillary
It is provided with flow control valve on sample feeding pipe, outlet port, the heating tube and the electricity are provided on the flow control valve
The connection of control system, the capillary sample feeding pipe, which inserts in the instant heating unit, obtains the gas to be analyzed that real time reaction generates,
The gas to be analyzed of the flow control valve control certain flow enters the quick mass spectrum from the capillary sample feeding pipe supervises online
Examining system, excessive gas are discharged by the outlet port；The heating of heating tube described in the electric control system controls, the heating
Pipe transfers heat to the capillary probe tube, and the insulating tube for being set to outer layer prevents thermal loss, and realization is described rapidly
The seamless connection of heating unit and the quick mass spectrum on-line monitoring system.
The quick mass spectrum on-line monitoring system, including probe tube, triple valve, cooling gas check valve B, ash content filter and fast
Fast mass spectrum on-line computing model；Gas to be analyzed is sampled after the special purpose interface by the probe tube, then passes through the threeway
Enter quick mass spectrum on-line computing model after valve, cooling gas check valve B and ash content filter.
The quick mass spectrum on-line monitoring system according to specific gas-solid reaction situation may be selected most fastly for 100 times/s not
Same frequency acquisition.
The electric-control system establishes communication connection by adjustable DC current regulator power supply and computer, forms Intelligent control electric
Source can set output power of the power supply in different moments, by computer software to realize instant heating unit in reaction process
In different heating rates and different heating final temperature requirement.
The temp measuring system includes thermocouple, thermocouple signal isolator, voltage amplifier and data acquisition module, described
Thermocouple obtains temperature data, through thermocouple signal isolator compensated chamber temperature difference, by the voltage amplifier by thermoelectricity
Even millivolt signal amplification, inputs the computer, the frequency acquisition of the data acquisition module by the data acquisition module
Most fastly it is 2000 times/s, realizes that reactant Millisecond reaction information in instant heating reaction process captures.
The thermocouple welding is on the center of the upper layer heating net, the thermocouple and the thermocouple and upper layer
The welding spot diameter of heating net is less than or equal to reactant particle diameter.
The upper layer heating net and lower layer's heating net are wire mesh or metallic film.
The rate of heat addition adjustable range of the instant heating unit is 1 DEG C/s~1000 DEG C/s.
The present invention compared to the prior art, have it is following the utility model has the advantages that
Silk screen instant heating of the present invention and quick mass spectrum gas-solid facies analysis instrument, which are realized, reacts reactant in instant heating
The high speed of the reaction informations such as instantaneous relase temperature, burst size and product component concentration of product component captures in the process, is intrinsic
Reaction kinetics research provide data basis.The design of simultaneous reactions instrument can effectively reduce the residence time of reaction product, drop
Low side reaction inhibits to extend influence, so that intrinsic characteristics of the reaction test closer to chemical reaction, obtain instant heating to be accurate
Gas-solid phase reaction mechanism and thermochemical process provide analysis means of testing in the process.
Detailed description of the invention
Fig. 1 is silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument schematic diagram of the invention.
Fig. 2 is silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument schematic diagram of the invention.
Fig. 3 (a) is the instant heating unit decomposition of silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument of the invention
Schematic diagram under state.
Fig. 3 (b) is after the instant heating unit of silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument of the invention assembles
Schematic diagram.
Fig. 4 is special purpose interface structural schematic diagram.
Fig. 5 (a)-Fig. 5 (d) is respectively 300 DEG C/s in embodiment 1,500 DEG C/s, 600 DEG C/s, the 800 DEG C/s rate of heat addition
Under temperature curve and Decomposition of Calcium Carbonate product CO2Formation curve.
Fig. 6 is 300 DEG C/s in embodiment 1,500 DEG C/s, 600 DEG C/s, Decomposition of Calcium Carbonate product under the 800 DEG C/s rate of heat addition
The curve comparison figure of CO2.
Fig. 7 be 300 DEG C/s in embodiment 1,500 DEG C/s, 600 DEG C/s, Decomposition of Calcium Carbonate converts under the 800 DEG C/s rate of heat addition
Rate comparison diagram.
Fig. 8 is 300 DEG C/s in embodiment 1,500 DEG C/s, 600 DEG C/s, calcium carbonate reaction rate under the 800 DEG C/s rate of heat addition
With conversion ratio graph of relation.
Fig. 9 (a)-Fig. 9 (e) be respectively in embodiment 1 react final temperature be 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C, 800 DEG C
When temperature curve and CO2Formation curve.
Figure 10 is the decomposition rate logarithm of calcium carbonate and the logarithmic relationship of conversion ratio under different heating final temperature in embodiment 1
Figure.
Figure 11 is the Decomposition of Calcium Carbonate reaction activity figure of calcium carbonate under different heating final temperature in embodiment 1.
Figure 12 (a)-Figure 12 (d) be respectively 8 DEG C/s in embodiment 2,45 DEG C/s, 120 DEG C/s, under the 300 DEG C/s rate of heat addition
Eucalyptus skin decomposition curve figure.
Appended drawing reference:
I, instant heating unit II, quick mass spectrum on-line monitoring system III, temp measuring system
IV, electric-control system V, special purpose interface
1, gas bomb 2, gas mass flow meter 3, gas mixer
4, cooling gas check valve A 5, triple valve 6, cooling gas check valve B
7, ash content filter 8, cooling gas check valve C 9, cooling gas check valve D
10, thermocouple 11, thermocouple signal isolator 12, high bandwidth isolating transmitter
13, data acquisition module 14, quick mass spectrum on-line computing model 15, adjustable DC current regulator power supply
16, computer 17, gas feed 18, heater lower end gas guiding channel
19, electrode 20, connecting wire 21, lower metal silk screen
22, pressing device 23, gas vent 24, thermocouple fixation hole
25, probe tube 26, upper layer wire mesh 27, sealing ring
28, hex bolts 29, cover of heater 30, capillary sample feeding pipe
31, heating tube 32, insulating tube 33, flow control valve
34, outlet port.
Specific embodiment
The contents of the present invention are described in further details with reference to the accompanying drawings and detailed description.
A kind of silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument, principle is as shown in Figure 1: with instant heating unit I
For core, heating power is controlled by electric-control system IV and then controls reaction heating rate and final temperature.Subparticle reactant is placed
Rapidly temperature reaction is carried out in instant heating unit I, the center that reaction composition granule is evenly distributed on lower metal silk screen 21 adds
Thermal region, gas conveying provide certain air velocity (0.1-1m/s) carrier gas or reaction gas, will be in heating reaction process
Real-time product a part enters quick mass spectrum on-line monitoring system II, realization product group in rapidly temperature-rise period to reaction product
Point instantaneous relase temperature, burst size and organize sub-sequence monitoring, it is ensured that the online capture of reaction information, and another part by
Gas vent discharge.By the real-time temperature collection data of temp measuring system III, different acquisitions is selected according to different heating conditions
Frequency, it can be achieved that 1-2000Hz temperature acquisition frequency.
As shown in Fig. 3 (a) and Fig. 3 (b), instant heating unit I, including cooling gas check valve D9, gas feed 17, heater
Lower end gas guiding channel 18, lower metal silk screen 21, upper layer wire mesh 26, pressing device 22, electrode 19 and connecting wire
20, sealing ring 27, cover of heater 29, wherein there are also thermocouple fixation hole 24, probe tube 25, gas vents 23 on cover of heater 29
With check valve A4.
Before test, reaction composition granule is uniformly placed on lower metal silk screen 21, and wire mesh both ends pass through pressing device
22 are clamped in two end electrodes, and electrode 19 is connected to electric-control system IV by connecting wire 20, are controlled and are heated by electric-control system IV
Power is to realize different heating requirement；It goes to the bottom on heater intermediate by 27 fixing seal of eight hex bolts 28 and sealing ring.
As shown in Fig. 2, the reaction gas or carrier gas when test in gas bomb 1 are entered under heater by gas feed 17
The flow-guiding channel 18 for holding gas is reacted with sample particle by heating silk screen 21 after gas flow rate is steady and (is taken when as carrier gas
Band and diluting reaction product), reaction product a part passes through probe tube 25,5 cooling gas check valve B4 of triple valve and ash content filter 7
Real-time product analysis is carried out into quick mass spectrum on-line computing model 14；Upper end gas vent 23 row of the another part from cover of heater
Out, exit, which fills a cooling gas check valve A4, prevents air from entering heater.The real time temperature of reaction particles is by being welded on upper layer silk
The thermocouple wire 10 at 26 center of net measures, and thermocouple connects temp measuring system progress real time data by thermocouple fixation hole 24 and adopts
Collection.
Gas is conveyed by gas bomb 1, gas mass flow meter 2, gas mixer 3, triple valve 5 and cooling gas check valve D9
Control；It requires to select different reaction gas or carrier gas according to specific experiments, gas controls each gas by gas mass flow meter 2
After body flow, reacted by lower metal silk screen 21 with sample particle after 3 mixed gas of gas mixer, then through dedicated
Enter quick mass spectrum on-line monitoring system II after interface V.
As shown in figure 4, special purpose interface V includes the capillary sample feeding pipe 30 set gradually from the inside to the outside, heating tube 31, heat preservation
Pipe 32 is provided with flow control valve 33 on capillary sample feeding pipe 30, outlet port 34, heating tube is provided on flow control valve
31 connect with electric-control system IV, and capillary sample feeding pipe 30, which inserts in instant heating unit I, obtains the gas to be analyzed that real time reaction generates
Body, the gas to be analyzed that flow control valve 33 controls certain flow enter quick mass spectrum on-line monitoring system from capillary sample feeding pipe 30
II, excessive gas is discharged by outlet port 34；Electric-control system IV controls heating tube 31 and heats, and heating tube 31 is by heat transfer
To capillary probe tube 30, the insulating tube 32 for being set to outer layer prevents thermal loss, realizes that instant heating unit I and quick mass spectrum exist
The seamless connection of line monitoring system II.
Quick mass spectrum on-line monitoring system II is released for monitoring reactant the instantaneous of product component in rapidly temperature-rise period
Put temperature, burst size and group sub-sequence, including probe tube 25, triple valve 5, cooling gas check valve B6, ash content filter 7 and quick matter
On-line computing model 14 is composed, quick mass spectrum on-line computing model 14 uses the mass spectrograph of model SPIMS-1000 in the present embodiment；It is anxious
Speed heating reaction product enters probe tube 25 after special purpose interface V, is filtered by triple valve 5, cooling gas check valve B6 and ash content
Device 7 enters quick mass spectrum on-line computing model 14 and carries out real-time data analysis, and cooling gas check valve B6 and ash content filter 7 prevent gas
The ash content that body water conservancy diversion and experiment generate enters mass spectrograph impact analysis.
Temp measuring system III for acquiring the temperature of reaction composition granule, including thermocouple 10, thermocouple signal isolator in real time
11, voltage amplifier 12, data acquisition module 13, computer 16；Thermocouple 10 is welded on to the center of upper layer wire mesh 26,
By 11 compensated chamber's temperature difference of thermocouple signal isolator, voltage amplifier 12 is accessed by thermocouple millivolt signal value and is amplified to number
According to the input value range of acquisition module 13, the temperature acquisition of different requirements may be implemented by the frequency acquisition of data acquisition module
Frequency.
The liter of main control instant heating unit I wire mesh 26 and lower metal silk screen 21 at the middle and upper levels of electric-control system IV
Warm parameter forms intelligent control function by adjustable DC current regulator power supply 15 and the connection of computer 16, passes through computer software
Output power of the power supply in different moments is set, to realize the rate of heat addition in reaction process and heat the control of final temperature.
The combination of instant heating unit I and quick mass spectrum on-line monitoring system II can be realized minimal diffusion effect and millisecond
Order reaction information capture effectively reduces the residence time of reaction product, and secondary response and side reaction is avoided to occur, and inhibits diffusion shadow
Ring so that intrinsic characteristics of the reaction test closer to chemical reaction, accurate simulation and during obtaining instant heating gas-solid it is opposite
Answer mechanism, thermochemical process.
The rapidly temperature data acquisition of temp measuring system III realizes the controllability frequency acquisition of 1-2000 times/s, quick matter
II reaction product is quickly pumped into mass spectrograph 14 by spectrum on-line monitoring system to be analyzed, and the speed of evacuation may be up to 5.3m/s, and maximum can
The residence time that can be reduced reaction product, secondary response is avoided, mass spectrograph can be according to the different acquisitions for requiring to realize different frequency
(0-100Hz, real-time display heat constituent, concentration and the flow of the product in reaction process, are able to achieve reactant and exist frequency
Rapidly Millisecond reaction information captures in transient prediction reaction process.
Silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument of the invention, using steps are as follows:
1) the response sample particle prepared is loaded among lower metal silk screen 21 and upper layer wire mesh 26, is made anti-
It answers composition granule to be evenly distributed on lower metal silk screen 21, theoretically, is generally evenly distributed in each microcosmic upper reaction composition granule
It on the surface of wire mesh, can integrally be heated to avoid reactant caused by particle agglomeration so unevenly, keep heating more equal
Even effectively composition granule is reacted in fixation that can be more stable using upper layer and lower layer wire mesh, reduces reaction gas (or carrier gas)
Particle is washed away；
2) heater is merged into sealing up and down, sealing ring 27 is equipped among upper and lower body can guarantee that reaction is in setting gas
It is reacted under body atmosphere；
3) reaction gas in gas bomb 1 or carrier gas are entered rapidly by gas mass flow meter 2, gas mixer 3
Heating unit I, the setting of gas flow size make the superficial gas flow in the instant heating unit I under reaction temperature be greater than by
The analysis gas flow that quick mass spectrum on-line computing model 14 is taken away from probe tube 25 opens 1 a period of time of gas bomb in advance,
Make in instant heating unit full of after reaction gas (or carrier gas)；
4) adjustable DC current regulator power supply 15 is opened, sets output work according to target heating rate and target heating final temperature
Rate；
5) mass spectrograph and temperature acquisition software on computer 16 are opened, records temperature of charge data and mass spectrograph in real time
Data change with time value；
6) it opens adjustable DC current regulator power supply 15 to begin to warm up, after reaching target temperature value according to target heating rate
Changing output power of power supply makes the control of wire mesh temperature in target temperature；
7) adjustment probe tube 25, reaction gas or carrier gas 1 and quick mass spectrum on-line monitoring after reaching the setting reaction time
Triple valve 5 between instrument 14, the connection that mass spectrograph and instant heating unit I is truncated build mass spectrograph with reaction gas (or carrier gas)
Found new air circuit connection；
8) Spectroscopy data acquisition and temperature data acquisition are closed, the measurement result of record is exported.
Specific application example of the invention
Example one
By typical gas-solid phase reaction --- for the thermal decomposition under calcium carbonate high temperature, illustrate specific embodiment party of the invention
Formula.
Calcium carbonate reagent is analyzed into pure (calcium carbonate content is no less than 99.0%) in the present embodiment, with national standard test sieve
The particle of 200-300 mesh (partial size is 48 microns -75 microns) is screened, and is weighed with the scientific balance of accuracy class d=0.1mg
10mg ± 0.5mg is homogeneously disposed among two layers of national standard 316L400 mesh stainless steel cloth, uses flow (pure for 3L/min High Purity Nitrogen
99.999%) degree washes away the gas that reaction generates in real time as carrier gas.The platinum-rhodium-platinum thermocouple that diameter is 75 microns is welded on
Stainless steel cloth center, make weld diameter control with react the same magnitude of composition granule, in actual experiment be believed that
The temperature value that thermocouple measurement is arrived is the temperature value for reacting composition granule.
The research of Decomposition of Calcium Carbonate characteristic under different heating rates.Adjust electric-control system set the rate of heat addition as 300 DEG C/
S, 500 DEG C/s, 600 DEG C/s, under 800 DEG C/s to same heating final temperature, pass through the reactant that temp measuring system and mass spectrograph obtain
The real time temperature data and CO of grain2Resolution characteristic such as Fig. 5 of the calcium carbonate under different heating rates can be obtained in instantaneous relase amount
(a) shown in-Fig. 5 (d), Fig. 6 is that rate of heat addition Decomposition of Calcium Carbonate at 300 DEG C/s, 500 DEG C/s, 600 DEG C/s, 800 DEG C/s produces
Object CO2Curve comparison figure.
It can be obtained by the Decomposition of Calcium Carbonate characteristic and traditional test means in instant heating by measurement result
The difference of the slow heat of such as TGA, and instant heating situation is extrapolated from the High Temperature Dissociation of Calcium Carbonate under different heating rates
Under reacting dynamics characteristic, disclose the intrinsic characteristics in practical chemical reaction, accurate gas-solid phase during understanding instant heating
Reaction mechanism, thermochemical process.
By CO under above four groups of different heating rates2Formation curve experimental data converge to obtain it is total as shown in Figure 6.
Conversion ratio is found out by formula (1) when Decomposition of Calcium Carbonate:
F is total gas flow rate in formula (1)；For CO in gas2Volume fraction,For CaCO3Sample introduction
Quality, the CO obtained from mass spectrograph2Volume fraction can calculate the conversion ratio curve under calcium carbonate different heating rates, similarly
Also under available different heating rates conversion ratio and reaction rate relationship.
Calcium carbonate pyrolysis conversion ratio under the different heating rates acquired according to above formula is as shown in fig. 7, from different heating speed
Calcium carbonate conversion ratio curve under rate can be seen that the increase with the rate of heat addition, and conversion ratio curve global slopes increase, carbonic acid
The time that calcium is converted completely significantly reduces, and the time point of start transition is shifted to an earlier date.
From the curve of reaction rate and conversion ratio under Fig. 8 different heating rates it can also be seen that the promotion of the rate of heat addition has
Conducive to reaction rate of quickening calcium carbonate during W-response, but the corresponding conversion ratio of maximum reaction rate point is increased
Greatly, under 300 DEG C/s, 500 DEG C/s, 600 DEG C/s, the 800 DEG C/s rate of heat addition, the corresponding conversion ratio size of maximum reaction rate according to
It is secondary are as follows: 0.38,0.41,0.42,0.45.
The research of Decomposition of Calcium Carbonate characteristic under different heating final temperature.Adjust electric-control system to 300 DEG C of the same rate of heat addition/
S is heated to 600 DEG C of different final temperatures, 650 DEG C, 700 DEG C, 750 DEG C, 800 DEG C, the reaction obtained by temp measuring system and mass spectrograph
The real time temperature data and CO2 instantaneous relase amount of composition granule, can be obtained the resolution characteristic of the calcium carbonate under different heating final temperature such as
Shown in Fig. 9 (a)-Fig. 9 (e).
It is changed with time relationship by Decomposition of Calcium Carbonate under different heating final temperature, reaction rate and conversion ratio can be calculated
Relation derivation kinetic simulation type function and apparent activation energy.Formula (2), (3) respectively represent reaction model function and Arrhenius
Equation:
K (T) is reaction rate constant at a temperature of T in formula (2), and A is pre-exponential factor in (3), and E is apparent activation energy.
After taking natural logrithm to formula (2), it is associated with the curve graph of experimental data under different temperatures and is fitted, because of power
That learns parameter asks calculation that the selection balance control stage is needed to carry out linear fit, and the fitted area of selection is -3 < ln (1-x) < -1
As shown in Figure 10.
It can be seen that the spy of the linear fit under different temperatures according to the associated diagram of Fig. 9 decomposition rate logarithm and conversion ratio logarithm
Property, can calculate the order of reaction, rate constant and the linear coefficient under each temperature decomposition condition, as a result as shown in figure 11, can be with
Find out that decomposition reaction of the calcium carbonate under the reaction unit just has good reproducibility, the order of reaction is between 0.75-0.78, root
The apparent activation energy of the reaction is found out according to its slope and intercept and pre-exponential factor is respectively 121.11kJ/mol and 806129s-1.
Decomposition of Calcium Carbonate gaseous product concentration and temperature are measured according to silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument
The activation energy that degree corresponding relationship acquires is significantly lower than the result of study of most of gas-solid reaction instrument, but in model reported in the literature
It encloses etc (120-280kJ/mol), general gas-solid reaction device, root is faster than with the reaction speed in instant heating device known to this
The kinetic simulation type function linearity extrapolated according to the data measured is good, and the order of reaction is almost the same at each temperature, this table
The kinetic parameter and mechanism model function of the bright quick mass spectrometer arrangement of instant heating are accurate and reliable.
As can be seen from FIG. 11 under different heating final temperature calcium carbonate Decomposition of Calcium Carbonate reaction activity.
Example two
By taking the thermal decomposition under biomass high-temperature as an example, the silk screen instant heating and quick mass spectrum gas that the present invention is further explained
Specific embodiment of the solid phase assays instrument in quick complex reaction.
Select Eucalyptus skin as canonical biometric matter in the present embodiment, Eucalyptus Pi Fenyong national standard test sieve screens 100-
The particle of 200 mesh (partial size be 75 microns -150 microns), and with the scientific balance of accuracy class d=0.1mg weigh 20mg ±
0.5mg is homogeneously disposed among two layers of national standard 316L300 mesh stainless steel cloth, uses flow for 3L/min high-purity argon gas (purity
99.999%) gas that reaction generates is washed away in real time as carrier gas.The platinum-rhodium-platinum thermocouple that diameter is 100 microns is welded on not
Become rusty steel wire center, make weld diameter control with react the same magnitude of composition granule, it is in actual experiment it is believed that hot
The temperature value that galvanic couple measures is the temperature value for reacting composition granule.
Adjust silk screen instant heating and the quick mass spectrum gas-solid facies analysis instrument rate of heat addition be 8 DEG C/s, 45 DEG C/s, 420 DEG C/
S, at 300 DEG C/s to same 700 DEG C of heating final temperature, the real time temperature number of reaction composition granule is obtained by temp measuring system and mass spectrograph
According to key product instantaneous relase amount, resolution characteristic such as Figure 12 (a)-Figure 12 of the Eucalyptus skin under different heating rates can be obtained
(d) shown in.It can be obtained by the biomass thermal resolution characteristic under different heating rates by measurement result, extrapolate instant heating
In the case of reacting dynamics characteristic.
Above-listed detailed description is illustrating for possible embodiments of the present invention, and the embodiment is not to limit this hair
Bright the scope of the patents, all equivalence enforcements or change without departing from carried out by the present invention, is intended to be limited solely by the scope of the patents of this case.
Claims (10)
1. a kind of silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: including instant heating unit (I),
Quick mass spectrum on-line monitoring system (II), temp measuring system (III) and electric-control system (IV), the instant heating unit (I) pass through special
Be seamlessly connected with interface (V) and the quick mass spectrum on-line monitoring system (II), subparticle reactant be placed on it is described rapidly
Rapidly temperature reaction is carried out in heating unit (I), the instant heating unit (I) is real under the control of the electric-control system (IV)
The requirement of existing different heating rates and different heating final temperatures, can get reaction by the quick mass spectrum on-line monitoring system (II)
Product component and concentration data obtain real-time reactant heating data by the temp measuring system (III).
2. silk screen instant heating according to claim 1 and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: the urgency
Fast heating unit (I) includes the heater body and heater upper cover (29) for placing subparticle reactant, the heating
The two sides of device ontology upper end are respectively arranged with electrode (19), and the electrode (19) of two sides is equipped with lower layer's heating net (21), described to add
Hot device upper cover (29) is equipped with upper layer heating net (26) and pressing device (22), and the pressing device (22) is by the upper layer heating net
(26) it is pressed in the electrode (19) with lower layer's heating net (21), the electrode (19) passes through conducting wire and the electric-control system (IV)
Connection.
3. silk screen instant heating according to claim 1 and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: described special
It include the capillary sample feeding pipe (30) set gradually from the inside to the outside, heating tube (31), insulating tube (32) with interface (V), in the hair
It is provided with flow control valve (33), is provided on the flow control valve outlet port (34) on thin sample feeding pipe (30), it is described
Heating tube (31) is connect with the electric-control system (IV), and the capillary sample feeding pipe (30) inserts in the instant heating unit (I)
Obtain the gas to be analyzed that real time reaction generates, the gas to be analyzed of the flow control valve (33) control certain flow is from described
Capillary sample feeding pipe (30) enters the quick mass spectrum on-line monitoring system (II), and excessive gas passes through the outlet port (34)
Discharge；The electric-control system (IV) controls heating tube (31) heating, and the heating tube (31) transfers heat to the hair
Thin probe tube (30), the insulating tube (32) for being set to outer layer prevent thermal loss, realize the instant heating unit (I) with
The seamless connection of the quick mass spectrum on-line monitoring system (II).
4. silk screen instant heating according to claim 1 and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: described fast
Fast mass spectrum on-line monitoring system (II), including probe tube (25), triple valve (5), cooling gas check valve B (6), ash content filter (7)
With quick mass spectrum on-line computing model (14)；Gas to be analyzed is taken after the special purpose interface (V) by the probe tube (25)
Sample, then quick mass spectrum on-line computing model is entered by the triple valve (5), cooling gas check valve B (6) and ash content filter (7) afterwards
(14)。
5. silk screen instant heating according to claim 4 and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: described fast
Fast mass spectrum on-line monitoring system (II) may be selected to be fastly most the different acquisition frequency of 100 times/s according to specific gas-solid reaction situation.
6. silk screen instant heating according to claim 1 and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: the electricity
Control system (IV) establishes communication connection by adjustable DC current regulator power supply (15) and computer (16), forms Intelligent control electric
Source can set output power of the power supply in different moments, by computer software to realize that instant heating unit (I) was reacting
The requirement of different heating rates and different heating final temperature in journey.
7. silk screen instant heating according to claim 6 and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: the survey
Warm system (III) includes thermocouple (10), thermocouple signal isolator (11), voltage amplifier (12) and data acquisition module
(13), the thermocouple (10) obtains temperature data, through thermocouple signal isolator (11) compensated chamber temperature difference, by described
Voltage amplifier (12) amplifies thermocouple millivolt signal, inputs the computer by the data acquisition module (13)
(16), the frequency acquisition of the data acquisition module (13) is most 2000 times/s fastly, realizes that reactant was reacted in instant heating
Millisecond reaction information captures in journey.
8. silk screen instant heating according to claim 7 and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: the heat
Galvanic couple (10) be welded on the center of the upper layer heating net (26), the thermocouple (10) and the thermocouple (10) with it is upper
The welding spot diameter of layer heating net (26) is less than or equal to reactant particle diameter.
9. silk screen instant heating according to claim 1 and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: on described
Layer heating net (26) and lower layer's heating net (21) is wire mesh or metallic film.
10. silk screen instant heating according to claim 1 and quick mass spectrum gas-solid facies analysis instrument, it is characterised in that: described
The rate of heat addition adjustable range of instant heating unit (I) is 1 DEG C/s~1000 DEG C/s.
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| Publication number | Priority date | Publication date | Assignee | Title |
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