CN206208830U - A kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis - Google Patents
A kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis Download PDFInfo
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- CN206208830U CN206208830U CN201621138313.4U CN201621138313U CN206208830U CN 206208830 U CN206208830 U CN 206208830U CN 201621138313 U CN201621138313 U CN 201621138313U CN 206208830 U CN206208830 U CN 206208830U
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- thermal decomposition
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Abstract
The utility model is related to a kind of atmospheric pressure photoionization mass spectrometric apparatus of on-line analysis solid fuel pyrolysis, and the device includes pyrolysis oven, auxiliary solvent flashing retraction mechanism, atmospheric pressure photoionization source and mass spectrograph.With the increasingly depleted of fossil fuel, the technique for preparing various hydrocarbon fuels and petrochemical materials by solid fuel pyrolysis is increasingly subject to the attention of people.The utility model can accurate quick on-line analysis solid waste（Such as polypropylene）, biomass, coal, solid fuel pyrolysis product species distribution and the formation mechanism such as oil shale, us can be helped preferably to grasp its pyrolysis inherent law, effective utilization of resource is realized comprehensively, to the sustainable development important in inhibiting of China.
Description
Technical field
The utility model belongs to the experimental technique in heat analysis field, and specifically one kind can quick and precisely real-time online
Analyze the atmospheric pressure photoionization mass spectrometric apparatus of solid fuel pyrolysis product.
Background technology
In recent years, the requirement based on using energy source and environmental protection, solid fuel thermochemical study is using by people
Attention, solid fuel pyrolysis are not only one kind of solid fuel Land use systems, and are also solid fuel ignition and gasified
The stage of Cheng Suobi warps, therefore it is particularly significant to carry out deep study mechanism to it.The pyrolytic process of solid fuel is extremely complex,
Product species are various, only accurately and comprehensively obtain the information of various stabilizations and unstable product, could profound understanding biomass
Pyrolysis mechanism.Mainly with thermogravimetric technology, application of gas chromatorgraphy/mass technology and low-voltage optical from mass spectrum in the Study on Pyrolysis of solid fuel
Based on technology.However, thermogravimetric technology can only be from the mass change for macroscopically obtaining solid fuel pyrolysis, and activation energy and reaction
The pyrolysis parameters of rock such as speed, but it is helpless to understanding the microprocess of solid fuel pyrolysis.Application of gas chromatorgraphy/mass is based on thermal decomposition product
The difference of boiling point or polarity simultaneously carries out qualitatively experimental technique according to the holdup time of component to product.In order to ensure higher dividing
From ability, the length of chromatographic column is generally 30-50 meters or so, causes disengaging time long, can only detect do not react, tool
There are the species of heat endurance, it is impossible to which the initial product to being pyrolyzed carries out quick, real-time analysis.Additionally, being adopted in application of gas chromatorgraphy/mass technology
Ionization mode is generally electron impact ionization, and electron impact ionization is " hard " ionization, can make thermal decomposition product species in ionization
During produce many fragment ions, determining for those compounds not efficiently separated in the chromatography column because property is close can be given
Property brings puzzlement.Compared to electron impact ionization, photo-ionisation is a kind of " soft " ionization, only produces molecular ion peak.Therefore, closely
Low-voltage optical has obtained increasingly being widely applied in analysis of the mass-spectrometric technique in solid fuel pyrolysis product over year（Y.
Wang, Q. Huang, Z. Zhou, Y. Pan, etal, Energy Fuels, 2015, 29, 1090 – 1098）.
But, low-voltage optical occurs in environment under low pressure from mass-spectrometric technique, to avoid not volatile component pollution cavity, general thermal decomposition product
Just enter in low-voltage vacuum chamber after must being filtered through filter disc, cause the relatively large product for being easier to condensation of quality to be analyzed inspection
Survey.Nonetheless, the relatively small product of many quality（m/z≤200）Can still be remained in vacuum cavity, pollute cavity.In order to
The cleaning of vacuum cavity is maintained, it is necessary to often clean instrument, it is cumbersome.However, atmospheric pressure photoionization is to utilize VUV
The ionization techniques that light source under atmospheric conditions ionizes gas phase sample, the big quality compounds that the technology can be produced to pyrolysis
Direct Analysis, while remaining the advantage of soft ionization that photo-ionisation possesses and nonpolarity discrimination.It is smaller for photoionization cross section
Compound, direct light ionizing efficiency is relatively low, can be carried by way of introducing volatility dopant in atmospheric pressure photoionization
Its ionizing efficiency high.
Utility model content
The purpose of this utility model is to provide a kind of atmospheric pressure photoionization mass spectrum for on-line analysis solid fuel pyrolysis
Device.
Specific technical scheme is as follows：
A kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis include pyrolysis oven, auxiliary volatilization
Solvent retraction mechanism, atmospheric pressure photoionization source and mass spectrograph；
The pyrolysis oven includes quartz sample boat 5, quartzy thermal decomposition tube 4 and pyrolysis mechanism；
One end of the quartzy thermal decomposition tube 4 is inlet end, and inlet end connects one end of the first carrier gas pipe 1；The other end is
The port of export, the port of export is located in cage 11；The quartz sample boat 5 is the sample feeding rod of channel-shaped, sample feeding rod it is inner by
The inlet end stretches into the middle part in quartzy thermal decomposition tube 4；The pyrolysis mechanism includes electrical heating wire, and the electrical heating wire is around being located at
On quartzy thermal decomposition tube 4；
The auxiliary solvent flashing retraction mechanism includes solvent flashing storage tank 22；The quartzy thermal decomposition tube adjacent with cage 11
4 side connects the outlet of the solvent flashing storage tank 22, and the side of solvent flashing storage tank 22 is provided with the 3rd carrier gas pipe 23, the
One end of three carrier gas pipes 23 is stretched under the solvent flashing liquid level in solvent flashing storage tank 22, and the other end is located at solvent flashing storage tank
Outside 22；
The atmospheric pressure photoionization source is located at the side of cage 11, and the light outlet in atmospheric pressure photoionization source is located at isolation
In cover 11, and light outlet is perpendicular to the port of export of quartzy thermal decomposition tube 4；The side in atmospheric pressure photoionization source is provided with the second carrier gas pipe
13, the outlet side of the second carrier gas pipe 13 is located at the side of the socket；
The mass spectrometric mass ions entrance 17 is located at the opposite side of cage 11；The bottom of cage 11 is provided with waste discharge
Gas port；
During for detecting, measured object is placed at the inner of sample feeding rod.
The technical scheme for further limiting is as follows：
The outlet diameter of quartzy thermal decomposition tube 4 is 2~4mm, and the middle part of quartzy thermal decomposition tube 4 is arranged with the first heater strip 7, with the
The corresponding quartzy thermal decomposition tube 4 of one heater strip 7 is provided with insulation material 6；Winding on the quartzy thermal decomposition tube 4 of thermal decomposition product outlet side
There is the second heater strip 12；The heat radiation of the first heater strip 7 thermally decomposes sample 9, and the heat radiation of the second heater strip 12 makes volatilization molten
Agent 21 is preheated and solvent flashing 21 is not condensed in quartzy thermal decomposition tube 4 after mixing with thermal decomposition product.
Be provided with thermocouple 8 outside the inner corresponding quartzy thermal decomposition tube 4 of sample feeding rod, thermocouple 8 is located at insulation material 6
It is interior.
The outlet of the solvent flashing storage tank 22 is provided with two-way valve 20, and heater strip is also arranged with outlet.
Connected on the first carrier gas pipe 1 first mass flow controller 2 and the first valve 3；The second carrier gas pipe
Connected on 13 second mass flow controller 14 and the second valve 15；Connected on the 3rd carrier gas pipe 23 the 3rd quality stream
The valve 25 of amount controller 24 and the 3rd.
The mass spectrograph be level Four bar mass analyzer or ion strap mass analyzer or flying time mass spectrum analysis device or
Orbit ion trap mass analyzer.
The atmospheric pressure photoionization source is VUV discharge lamp or argon lamp or krypton lamp or xenon lamp or hydrogen lamp.
The port of export of the quartzy thermal decomposition tube 4 parallel to mass ions entrance 17, and vertical range between the two for 2~
6mm。
Advantageous Effects of the present utility model embody in the following areas：
1. relatively easy, pretreatment process and the chromatographic isolation such as thermal decomposition product is without collecting, extraction are operated, can be quickly real-time
Analysis detection pyrolysis initial product.
2. this " soft " ionization technique of atmospheric pressure photoionization causes that thermal decomposition product species are ionized rear fragment ion relatively
Few, product peak is relatively easy, is easy to carry out qualitative analysis to thermal decomposition product.
3. thermal decomposition product needs not move through filter disc, and the thermal decomposition product of big quality can also be analyzed directly so that institute's calorimetric solution
The mass distribution range of product is wider.
4. thermal decomposition product is to be ionized in atmospheric pressure environment such that it is able to quick, real-time detection pyrolysis initial product species
Distribution, has extremely important scientific meaning to research pyrolysis mechanism.
Brief description of the drawings
Fig. 1 is the utility model structural representation.
Fig. 2 be positive ion mode under, do not introduce solvent flashing, cellulose powder（Particle diameter：50µm）In 400 °C of pyrolysis matter
Spectrogram.
Fig. 3 be positive ion mode under, introduce solvent flashing toluene gas, cellulose powder（Particle diameter：50µm）At 400 °C
Pyrolysis mass spectrogram.
Fig. 4 be positive ion mode under, do not introduce solvent flashing, polypropylene powder（Superfine chemical is pure）In 600 °C of pyrolysis
Mass spectrogram.
Sequence number in Fig. 1：Carrier gas pipe 1, the first mass flow controller 2, the first valve 3, quartzy thermal decomposition tube 4, quartz sample
Boat 5, insulation material 6, the first heater strip 7, thermocouple 8, sample 9, temperature controller 10, cage 11, the second heater strip 12, second are carried
Tracheae 13, the second mass flow controller 14, the second valve 15, atmospheric pressure photoionization source 16, mass ions entrance 17, ion are passed
Defeated pipe 18, dry gas 19, two-way valve 20, solvent flashing 21, solvent flashing storage tank 22, the 3rd carrier gas channel 23, the 3rd flow control
Device processed 24, the 3rd valve 25.
Specific embodiment
Below in conjunction with the accompanying drawings, by embodiment, the utility model is further described.
Referring to Fig. 1, a kind of atmospheric pressure photoionization mass spectrometric apparatus of on-line analysis solid fuel pyrolysis include pyrolysis oven, auxiliary
Solvent flashing retraction mechanism, atmospheric pressure photoionization source and mass spectrograph.
Pyrolysis oven includes quartz sample boat 5, quartzy thermal decomposition tube 4 and pyrolysis mechanism；One end of quartzy thermal decomposition tube 4 is air inlet
End, inlet end connects one end of the first carrier gas pipe 1；The other end is the port of export, and the port of export is located in cage 11；Quartz sample
Boat 5 is the sample feeding rod of channel-shaped, and the inner of sample feeding rod is stretched into the middle part in quartzy thermal decomposition tube 4 by the inlet end, with sample feeding rod
Thermocouple 8 is provided with outside inner corresponding quartzy thermal decomposition tube 4, thermocouple 8 is located in insulation material 6.Pyrolysis mechanism includes that electricity adds
Heated filament, electrical heating wire is around being located on quartzy thermal decomposition tube 4.The outlet diameter of quartzy thermal decomposition tube 4 is, the middle part of quartzy thermal decomposition tube 4 around
Equipped with the first heater strip 7, the heat radiation of the first heater strip 7 thermally decomposes sample 9；With the corresponding quartz pyrolysis of the first heater strip 7
Pipe 4 is provided with insulation material 6；Around equipped with the second heater strip 12, the second heating on the quartzy thermal decomposition tube 4 of thermal decomposition product outlet side
The heat radiation of silk 12 preheats solvent flashing 21 and makes solvent flashing 21 not cold in quartzy thermal decomposition tube 4 after mixing with thermal decomposition product
It is solidifying.
Auxiliary solvent flashing retraction mechanism includes solvent flashing storage tank 22；The quartzy thermal decomposition tube 4 adjacent with cage 11
Side connects the outlet of the solvent flashing storage tank 22, and the outlet of solvent flashing storage tank 22 is provided with two-way valve 20, in outlet also
It is arranged with heater strip；The side of solvent flashing storage tank 22 is provided with the 3rd carrier gas pipe 23, and one end of the 3rd carrier gas pipe 23 stretches to waves
Under solvent flashing liquid level in hair solvent tank 22, the other end is located at outside solvent flashing storage tank 22.
Atmospheric pressure photoionization source is VUV discharge lamp 16, positioned at the side of cage 11, atmospheric pressure photoionization source
Light outlet is located in cage 11, and light outlet is perpendicular to the port of export of quartzy thermal decomposition tube 4；The one of atmospheric pressure photoionization source
Side is provided with the second carrier gas pipe 13, and the outlet side of the second carrier gas pipe 13 is located at the side of the socket；
Connected on first carrier gas pipe 1 first mass flow controller 2 and the first valve 3；Connected on second carrier gas pipe 13
The second mass flow controller 14 and the second valve 15；Connected on 3rd carrier gas pipe 23 He of the 3rd mass flow controller 24
3rd valve 25.
First mass flow controller 2, the second mass flow controller 14 and the 3rd mass flow controller 24 are matter
Amount flow controller；First valve 3, the second valve 15 and the 3rd valve 25 are stop valve.
Mass spectrometric mass ions entrance 17 is located at the opposite side of cage 11；The bottom of cage 11 is provided with waste air
Mouthful；Mass spectrograph is TOF.
The port of export of quartzy thermal decomposition tube 4 is parallel to mass ions entrance 17, and vertical range between the two is 4mm.
During for detecting, measured object is placed at the inner of sample feeding rod.
Operation principle of the present utility model is described as follows：
Referring to Fig. 1, solvent flashing storage tank 22 is built with solvent flashing 21, one end immersion solvent flashing 21 of carrier gas channel 23
Under liquid level；The 3rd valve 25 on the carrier gas channel 23 of two-way valve 20 and the 3rd is opened, by the 3rd on the 3rd carrier gas channel 23
The flow that the regulation and control solvent flashing of mass flow controller 24 is introduced.
The second valve 15 on the second carrier gas pipe 13 is opened, by the second mass flow controller on the second carrier gas pipe 13
14 regulate and control the flow of carrier gas.
First, the first heater strip 7 obtains electric, and quartzy thermal decomposition tube 4 is heated to pyrolysis temperature, opens mass spectrograph, opens vacuum purple
Outer discharge lamp 16, quartz sample boat 5 is placed in by sample 9, and the second heater strip 12 obtains electric, the 3rd mass flow controller 24 of opening,
3rd valve 25, the second mass flow controller 2 and the second valve 3, adjust carrier gas -1 and carrier gas -3, and thermal decomposition product and volatilization are molten
Agent 21 is wrapped up after converging in the port of export of quartzy thermal decomposition tube 4 in the presence of carrier gas -1 and carrier gas -3 respectively into cage 11
The atmospheric pressure photoionization area for coming, vacuum ultraviolet ionized, the ion of generation subsequently enters mass spectrograph and is detected analysis.
Referring to Fig. 2, the first heater strip 7 it is electric, quartzy thermal decomposition tube 4 is heated to 400 °C, the quartzy outlet of thermal decomposition tube 4 of regulation and
The temperature of the outlet of solvent flashing storage tank 22 is 250 °C, opens the second valve 15, will be carried by the second mass flow controller 14
Gas -2（Experiment carrier gas used is nitrogen）Flow set be 300sccm, the cellulose of sample 9 is placed in quartz sample boat 5, open
First valve 3, by the first mass flow controller 2 by the flow set of carrier gas -1 be 200sccm, thermal decomposition product is in carrier gas -1
In the presence of the atmospheric pressure photoionization area that is wrapped up into cage 11 by the port of export of quartzy thermal decomposition tube 4, it is purple by vacuum
Outer electric discharge krypton lamp 16 is ionized, the ion of generation then in the presence of electric field and pressure differential, by mass ions entrance 17 and from
Sub- transfer tube 18 enters the TOF in vacuum system and is detected analysis.Fig. 2 is obtained with the method
The mass spectrogram of cellulose pyrolytic product species distribution, major pyrolytic product such as furfural（m/z97.03）, 5- methyl-2-furfurals（m/
z111.04）, levoglucosenone（m/z127.04）, 3,5- dihydroxy -2- methyl -4H- pyranone（m/z143.03）, it is left-handed
Glucan（m/z163.04）Deng can be detected.
Referring to Fig. 3, the valve 25 of two-way valve 20 and the 3rd is opened, by the 3rd mass flow controller 24 by the stream of carrier gas -3
Amount is set to 40sccm, thermal decomposition product and solvent flashing 21（Experiment solvent flashing used is toluene）Respectively in carrier gas -1 and load
The port of export in the presence of gas -3 in quartzy thermal decomposition tube 4 enters the atmospheric pressure photoionization area that cage 11 is wrapped up after converging,
Ionized by VUV electric discharge krypton lamp 16, the ion of generation subsequently enters the TOF quilt in vacuum system
Detection and analysis.Other operations are with case 1.Fig. 3 is the mass spectrogram of the cellulose pyrolytic product species distribution obtained with the method, can
See that cellulose pyrolytic product species can be detected by quick and precisely real-time online, such as furfural（m/z97.03）, 5- methyl-2-furfurals
（m/z111.04）, levoglucosenone（m/z127.04）, 3,5- dihydroxy -2- methyl -4H- pyranone（m/z143.03）, it is left
Rotation glucan（m/z163.04）.After adding solvent flashing to be dopant toluene, the relative intensity of Some Species substantially increases, this
It is because toluene ion and thermal decomposition product occur ion molecule reaction so that the latter's intensity is significantly improved.
Referring to Fig. 4, the first heater strip 7 obtains electric, and quartzy thermal decomposition tube 4 is heated to 600 °C, and sample 9 is changed makees polypropylene PP, other
Operation is with case 1.Fig. 4 is the mass spectrogram of the polypropylene thermal decomposition product species distribution obtained with the method, can Real Time Observation to single
Alkene（M/z57.07, m/z 71.09 etc.）, alkadienes（M/z69.07, m/z83.09, m/z97.10 etc.）, alkatrienes（m/
z81.07、m/z 95.09、m/z 109.10、m/z 123.12、m/z137.13、m/z151.15、m/z165.16、m/
Z207.21, m/z249.26, m/z277.29 etc.）Deng major pyrolytic product.
Claims (7)
1. a kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis, it is characterised in that：Including pyrolysis
Stove, auxiliary solvent flashing retraction mechanism, atmospheric pressure photoionization source and mass spectrograph；
The pyrolysis oven includes quartz sample boat（5）, quartzy thermal decomposition tube（4）With pyrolysis mechanism；
The quartzy thermal decomposition tube（4）One end be inlet end, inlet end connects the first carrier gas pipe（1）One end；The other end is
The port of export, the port of export is located at cage（11）It is interior；The quartz sample boat（5）Be the sample feeding rod of channel-shaped, sample feeding rod it is interior
End quartzy thermal decomposition tube is stretched into by the inlet end（4）Interior middle part；The pyrolysis mechanism includes electrical heating wire, the electrical heating wire
Around being located at quartzy thermal decomposition tube（4）On；
The auxiliary solvent flashing retraction mechanism includes solvent flashing storage tank（22）；With cage（11）Adjacent quartzy thermal decomposition tube
（4）Side connect the solvent flashing storage tank（22）Outlet, solvent flashing storage tank（22）Side be provided with the 3rd carrier gas
Pipe（23）, the 3rd carrier gas pipe（23）One end stretch to solvent flashing storage tank（22）Under interior solvent flashing liquid level, other end position
In solvent flashing storage tank（22）It is outside；
The atmospheric pressure photoionization source is located at cage（11）Side, the light outlet in atmospheric pressure photoionization source is located at cage
（11）It is interior, and light outlet is perpendicular to quartzy thermal decomposition tube（4）The port of export；The side in atmospheric pressure photoionization source is provided with the second carrier gas
Pipe（13）, the second carrier gas pipe（13）Outlet side be located at socket side；
The mass spectrometric mass ions entrance（17）Positioned at cage（11）Opposite side；Cage（11）Bottom be provided with row
Exhaust outlet；
During for detecting, measured object is placed at the inner of sample feeding rod.
2. a kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis according to claim 1,
It is characterized in that：Quartzy thermal decomposition tube（4）Outlet diameter be 2~4mm, quartzy thermal decomposition tube（4）Middle part be arranged with the first heating
Silk（7）, with the first heater strip（7）Corresponding quartzy thermal decomposition tube（4）It is provided with insulation material（6）；Thermal decomposition product outlet side
Quartzy thermal decomposition tube（4）On be arranged with the second heater strip（12）；First heater strip（7）Heat radiation make sample（9）Thermal decomposition；Second
Heater strip（12）Heat radiation make solvent flashing（21）Preheat and make solvent flashing（21）In quartzy heat after mixing with thermal decomposition product
Xie Guan（4）In do not condense；
With the inner corresponding quartzy thermal decomposition tube of sample feeding rod（4）Outside is provided with thermocouple（8）, thermocouple（8）Positioned at insulation material
（6）It is interior.
3. a kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis according to claim 1,
It is characterized in that：The solvent flashing storage tank（22）Outlet be provided with two-way valve（20）, heater strip is also arranged with outlet（12）.
4. a kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis according to claim 1,
It is characterized in that：The first carrier gas pipe（1）On connect the first mass flow controller（2）With the first valve（3）；Described
Two carrier gas pipes（13）On connect the second mass flow controller（14）With the second valve（15）；The 3rd carrier gas pipe（23）On
Connect the 3rd mass flow controller（24）With the 3rd valve（25）.
5. a kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis according to claim 1,
It is characterized in that：The mass spectrograph is level Four bar mass analyzer or ion strap mass analyzer or flying time mass spectrum analysis device
Or orbit ion trap mass analyzer.
6. a kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis according to claim 1,
It is characterized in that：The atmospheric pressure photoionization source is VUV discharge lamp or argon lamp or krypton lamp or xenon lamp or hydrogen lamp.
7. a kind of atmospheric pressure photoionization mass spectrometric apparatus for on-line analysis solid fuel pyrolysis according to claim 1,
It is characterized in that：The quartzy thermal decomposition tube（4）The port of export parallel to mass ions entrance（17）, and between the two it is vertical away from
From being 2 ~ 6mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106324074A (en) * | 2016-10-20 | 2017-01-11 | 中国科学技术大学 | Atmospheric pressure photoionization mass spectrum device for analyzing solid fuel pyrolysis on line |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106324074A (en) * | 2016-10-20 | 2017-01-11 | 中国科学技术大学 | Atmospheric pressure photoionization mass spectrum device for analyzing solid fuel pyrolysis on line |
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