CN109557039A - The super-narrow line width infrared absorption spectrum measurement apparatus and method that gsec is differentiated - Google Patents
The super-narrow line width infrared absorption spectrum measurement apparatus and method that gsec is differentiated Download PDFInfo
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- 238000005259 measurement Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 32
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 17
- 230000003595 spectral effect Effects 0.000 claims abstract description 10
- 238000000691 measurement method Methods 0.000 claims abstract description 8
- 230000003287 optical effect Effects 0.000 claims description 22
- 230000001052 transient effect Effects 0.000 claims description 10
- 238000002835 absorbance Methods 0.000 claims description 9
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 8
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- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims description 3
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
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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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
Abstract
The present invention relates to the super-narrow line width infrared absorption spectrum measurement device and method that gsec is differentiated, for detecting the intermediate species of situ catalytic reaction.Device includes main control computer, temperature control module, modulation power source module, diode laser, light path system and locking phase detector；Measurement method is, by adjusting temperature and electric current, the pulse laser that modulation diode laser issues；Locking phase detector one end receives reference light, and one end receives the detection light from sample, converts after locking phase is handled to absorption spectrum.For the present invention using diode laser as probe source, spectral resolution is up to 0.0001nm, has been inherently eliminated spectra overlapping between different plant species, tells the various species occurred in catalytic reaction process so as to highly sensitive.Furthermore unique Phase Lock Technique is used, temporal resolution is not only increased to 10 μ s, so as to the short life centre species occurred during detection reaction, and Infrared jamming caused by reaction in-situ high temperature can be prevented.
Description
Technical field
The present invention relates to a kind of infrared absorption spectrum measurement device and method with ultraspectral resolution ratio, especially pass through
After phase lock amplifying technology, the temporal resolution of 10 μ s may be implemented.
Background technique
The alkene such as ethylene and propylene are important the raw material of wilderness demand in petroleum chemicals and national economy production.It is raw
The traditional handicraft for producing alkene is naphtha first to be produced from petroleum, then olefin feedstock is produced from naphtha.And petroleum refining per ton
The ratio of naphtha only has 15%-20% in product processed.China is the country an of oil starvation and few gas, is produced with traditional handicraft
The alkene such as ethylene and propylene, China lack certain advantage in raw material supply.But coal is that China is true in world energy sources structure
Positive dominant energy resources, explored coal reserves account for about the 11% of world saving.It is come into effect from the 1980s
After the national strategy of " with coal for replacing oil ", the scientific and technical personnel Creative Science and Technology Co. Ltd of Dalian Chemical Physics Research Institute --- from coal via methanol system
Low-carbon alkene is taken, the restriction of acquisition can only be refined from petroleum by changing low-carbon alkene raw material, will be become " with coal for replacing oil " by dream
For reality, methanol-to-olefins (MTO) industrialization production is realized, is persistently held the lead in the world.However during MTO
Mechanism of catalytic reaction, deactivation mechanism etc. still do not get across completely, many basic problems are not answered, these machines
Unknown in reason limits the development of MTO technology, therefore there is an urgent need to high-resolution spectral techniques to the centre in catalysis reaction
Product is distinguished.
In organic molecule, the atom of constitutional chemistry key or functional group goes out the state constantly vibrated and rotated, vibration
The range of dynamic frequency is in infrared light region.It is equal with the vibration of molecule or rotational frequency when incident infrared light frequency, and
When the vibration dipole moment of molecule changes, the chemical bond of intramolecular or functional group are absorbed by incident infrared light.Due to group
There is the characteristic absorption of oneself at the various groups of molecule, therefore infrared spectroscopy is a kind of hand that judgement molecular structure is very strong
Section, is widely used in agricultural, food, petrochemical industry, environment, medicine and other fields.Current commercialized infrared spectrometer mainly has
Two kinds, first is that using grating as the color dispersion-type infrared absorption spectrometer of dispersion original part, such as the SM301/SM301- of SP company, the U.S.
EX mid-infrared light spectrometer, the dual-beam infrared spectrophotometer of Chinese Tuo Pu company；Second is that FTIR technique
Instrument, such as the Spectrum Two infrared spectrometer of PerkinElmer company, the U.S., the Fourier transformation of Chinese Shimadzu Corporation are red
External spectrum instrument IRTrace-100.The light source of these infrared absorption spectrometers is all xenon source, spectral resolution in 1nm or more,
Temporal resolution is in 100us or more.For carry out situ catalytic repercussion study, spectral resolution can not eliminate different plant species it
Between spectra1 interfer-, and its temporal resolution cannot detect catalysis reaction intermediate species.
Summary of the invention
In view of the deficiencies of the prior art, in order to the intermediate species progress high-resolution detection to MTO catalysis reaction, this hair
It is bright to provide a kind of transient state infrared absorption spectrum experimental provision and measurement method with super-narrow line width.
Technical solution is as follows: the super-narrow line width transient state infrared absorption spectrum measurement device that gsec is differentiated, including master control
Computer, temperature control module, modulation power source, diode laser, light path system and locking phase detector；
The main control computer sends current order to modulation power source (3) for sending heat command to temperature control module, and
Time-resolved FTIR spectroscopy is shown according to the different moments absorbance from locking phase detector；
The temperature control module, for adjusting the temperature of frequency-doubling crystal in diode laser, thus change its microstructure,
And then adjust the wavelength of transmitting；
The modulation power source, for sending current signal to diode laser according to current order；
The diode laser, for exporting modulation laser signal extremely according to the relationship of temperature, electric current and wavelength, frequency
Light path system；
The light path system is divided into two parts for that will modulate laser signal, and a part enters lock as reference optical signal
One input port of phase detector, as detection light after sample bin, another into locking phase detector inputs another part
Mouthful；
Locking phase detector is sent to master control electricity for collecting reference optical signal and detection light, and by different moments absorbance
Brain.
The central wavelength scanning range of the diode laser emission is 1-2nm, spectral line width 0.0001nm.
The adjustable temperature range of the temperature control module is -5 DEG C~30 DEG C.
The sample bin uses molecular sieve tabletting sample preparation, and laser is made to carry out multiple reflections in sample, and signal carries out gain.
The reference optical signal is equal with detection light light intensity.
The super-narrow line width infrared absorption spectrum measurement method that gsec is differentiated, comprising the following steps:
(1) tabletting sample preparation after mixing sample with molecular sieve, is put into sample bin；
(2) main control computer is by the adjusting to temperature and electric current, and to the wavelength of laser, frequency and phase are modulated, and makes
Diode laser issues modulation laser signal；
(3) for modulation laser signal after light path system, reflective portion is directly entered locking phase detector, becomes reference light letter
Number；Transmissive portion is directly entered sample bin, and situ catalytic reaction occurs in sample bin, and the intermediate species of generation carry out detection light
It absorbs, is finally incident on locking phase detector, becomes detection optical signal；
(4) locking phase detector collects reference light and detection light, and the absorbance of different moments is passed to main control computer,
Show time-resolved infrared absorption spectrum.
The main control computer is by the adjusting to temperature and electric current, and to the wavelength of laser, frequency and phase are modulated packet
Include following steps:
It is calculated according to vibration level and the structural analysis of substance, obtains the range of the infrared absorption peak of intermediate species, and with
This is reference, adjusts the output wavelength of laser；
Using the temperature of diode laser, electric current and wavelength, the relationship of frequency, the wavelength according to needed for sample and in advance
The frequency and phase of setting obtain corresponding temperature value, current value；
Temperature value, current value are converted into heat command respectively by main control computer, current order is sent to temperature control module and tune
Power supply processed.
When reference optical signal is equal with detection light light intensity, pass through formulaObtain the suction of test substance
Luminosity, A indicate absorbance, IReference light、IDetect lightRespectively indicate reference optical signal and detection light.
It according to time-resolved infrared absorption spectrum, is fitted by data, obtains the intermediate species service life.
Traditional infrared spectrum technology, since its spectral resolution is low, in 1nm or more, while temporal resolution is greater than 100
μ s does not simply fail to eliminate resolution capability caused by the spectra overlapping of different plant species in catalysis reaction and declines, and can not detect
Intermediate species of the service life occurred in reaction in tens musec orders.Which results in can not react machine to situ catalytic all the time
The deep understanding of reason, to limit the further promotion of catalytic efficiency.The present invention is using diode laser as detection light
Source, spectral resolution are up to 0.0001nm, spectra overlapping between different plant species have been inherently eliminated, so as to highly sensitive
Tell the various species occurred in catalytic reaction process.Furthermore unique Phase Lock Technique is used, not only by temporal resolution
10 μ s are increased to, so as to the short life centre species occurred during detection reaction, and reaction in-situ height can be prevented
Infrared jamming caused by temperature.The present invention probes into the strong technological means of mechanism of catalytic reaction by becoming, so that catalysis be pushed to lead
The further development in domain.
Detailed description of the invention
Principle schematic diagram Fig. 1 of the invention.
Wherein, 1 main control computer, 2 adjustable thermostatic modules, 3 power modules, 4 diode lasers, 5 beam splitting systems, 6 samples
Storehouse, 7 locking phase detectors.
Fig. 2 measurement result of the present invention envisions schematic diagram.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
The present invention relates to the super-narrow line width infrared absorption spectrum measurement settings that a kind of gsec is differentiated, for detecting original position
It is catalyzed the intermediate species of reaction.Using Phase Lock Technique, after thermal module and power modulation, diode laser is issued
The super-narrow line width tuning laser beam of 0.0001nm, after beam splitting chip, a part of locking phase detector of directly entering makes reference light, in addition
A part enters reaction in-situ sample cell, after repeatedly penetrating molecular sieve press sheet compression, into locking phase detector as signal
Light.By specially designed lock-in amplifier technology, not only detection light intensity decays to mW magnitude (can be reduced into reaction high temperature
Caused Infrared jamming), the temporal resolution of 10 μ s can also be realized, thus the short life species in detection reaction.It is measured
Method is, by adjusting temperature and electric current, the laser that modulation diode laser issues；Locking phase detector one end receives reference
Light, one end receive the detection light from sample, convert after locking phase is handled to absorption spectrum.
As shown in Figure 1, the super-narrow line width infrared absorption spectrum measurement device that gsec is differentiated, diode laser are fixed
It is connected in high precision temperature control module, while with modulation power source；Optical path system is equipped among diode laser and locking phase detector
System and sample cell.Main control computer is connected to thermal module, modulation power source and locking phase detector simultaneously.
The excitation light source used in technology is diode laser, and the line width issued is generally 0.0001nm, is swashed
Light device central wavelength can be tuned by temperature and Injection Current, and scanning range is 1-2nm.
By Phase Lock Technique, using thermal module and power module, the laser issued to diode laser is modulated,
Luminous intensity is detected when measurement can decay to mW magnitude.It is acquired using locking phase detector as data, it, can be in conjunction with Phase Lock Technique
Realize the temporal resolution of 10 μ s.
Using semi-transparent semi-reflecting lens as beam splitting system, a part of light is directly entered locking phase detector as reference light, another
Part light enters sample bin.Optical path may be implemented in sample using molecular sieve tabletting sample preparation for transmission-type sample bin in sample bin
Multiple reflections.
Main control computer connects modulation power source module, high precision temperature control module, locking phase detector by governor circuit simultaneously.Two
Pole pipe laser is fixed on high-precision temperature control module, and modulation power source gives diode laser Injection Current signal, diode
The spectral line width of laser can reach 0.0001nm, laser center wavelength tuning range 1-2nm, so as to eliminate not jljl
The interference of spectrum between kind, and high-precision spectral resolution can detect the fine structure of absorption peak, provide more about vibration
Dynamic and rotational energy level information.By thermal module and power module, the frequency and phase of laser can be modulated, issues modulated signal
I.It passes through beam splitting chip, and a part is directly entered locking phase detector, becomes reference optical signal II；Another part enters sample in situ
Storehouse, using molecular sieve tabletting sample preparation, laser carries out multiple reflections in sample, and signal carries out gain, eventually enters into locking phase detection
Device becomes detection optical signal III.Locking phase detector detects light III and is collected to reference light II, and passes throughIt is converted into time-resolved INFRARED SPECTRUM, passes to main control computer.Based on locking phase
The temporal resolution of 10us may be implemented in amplifier technique and power technology, so as to detect the short life in reaction in-situ
Intermediate species.It, can be by detection light intensity decays to mW amount while guaranteeing certain signal-to-noise ratio meanwhile using Phase Lock Technique
Grade, and non-contact measurement, fundamentally prevent Infrared jamming caused by reaction in-situ high temperature.
The super-narrow line width transient state infrared absorption spectrum measurement method that gsec is differentiated is as follows:
(1) tabletting sample preparation after mixing sample with molecular sieve, is put into sample bin；
(2) software is utilized, by the adjusting to temperature and electric current, to the wavelength of laser, frequency and phase are modulated,
Diode laser is set to issue modulation laser signal I；
(3) for laser after beam splitting chip, a part is directly entered locking phase detector, becomes reference optical signal (II)；
(4) another light beam is directly entered sample bin, and situ catalytic reaction, the intermediate species pair of generation occur in sample bin
Detection light is absorbed, and locking phase detector is finally incident on, and becomes detection optical signal III；
(5) locking phase detector collects reference light I and detection light III, passes throughCalculate extinction
The data that different time acquires are passed to main control computer, show time-resolved infrared absorption spectrum by degree.
Diode laser is fixed in high-precision thermostat module, the temperature of thermostat module by semiconductor cooler come
It adjusts, and negative-feedback signal is provided to semiconductor cooler, to realize high-precision constant temperature as detection using thermistor
Control.Adjustable temperature range: the power supply 3 of -5 DEG C of -30 DEG C of main control computers 1 connection modulation, the current signal issued inject two poles
Pipe laser 4 adjusts excitation wavelength.The central wavelength scanning range 1-2nm that diode laser 4 emits, breadth of spectrum line
0.0001nm.Temperature and electric current are adjusted, also the frequency and phase of adjustable laser.The laser signal I modulated is provided with spy
Different " mark " (frequency and phase with setting), is incident on beam splitting system 5, and light-splitting device uses semi-transparent semi-reflecting lens, and one
Part light is directly entered a receiver section of locking phase detector 7, and as reference optical signal II, another light beam enters sample bin 6.To
Sample is put into molecular sieve and carries out tabletting sample preparation, detects light multiple reflections in sample bin 6, eventually enters into locking phase detector 7
Another end-receiver becomes detection optical signal III.Based on Phase Lock Technique, only there is the signal quilt of special " mark " of modulation
It collects, that is, the laser being only really absorbed by the sample is selected, to eliminate since the high temperature of reaction in-situ is led
The Infrared jamming of cause.Every 10 μ s most can be achieved fastly and acquire a data for modulation through Phase Lock Technique, therefore it is anti-to differentiate catalysis
Species among short life during answering.
Fig. 2 shows the experimental measurements of anticipation.Before measurement, laser signal I is modulated first, selection is suitable
Optical maser wavelength, frequency and phase.Then it is not put into sample, is measured, i.e., school zero is carried out to instrument.Later by sample with point
It is put into sample bin 6 after son sieve mixed pressuring plate sample preparation, is measured.Time of measuring scale can be from microsecond to second.Exist for the service life
The intermediate species of tens musec orders, with the progress of catalysis reaction, apparatus of the present invention can detect its characteristic absorption signal
First increase the process to decay afterwards.For the service life in the intermediate species of millimeter magnitude, the rising and decaying of signal can be in millimeters
Magnitude detects.For the product of catalysis reaction, it will detecting its characteristic absorption is constantly enhancing, and finally tends to constant letter
Number feature.Therefore the change curve decayed at any time based on the signal measured, it is available by carrying out data fitting to it
The service life of species to be measured.Apparatus of the present invention are to detect the strong means of situ catalytic reaction intermediates kind, to catalytic mechanism
Research will play an important role.
Claims (9)
1. the super-narrow line width transient state infrared absorption spectrum measurement device that gsec is differentiated, it is characterised in that including main control computer
(1), temperature control module (2), modulation power source (3), diode laser (4), light path system (5) and locking phase detector (7)；
The main control computer (1) sends current order to modulation power source (3) for sending heat command to temperature control module (2),
And time-resolved FTIR spectroscopy is shown according to the different moments absorbance from locking phase detector (7)；
The temperature control module (2), for adjusting the temperature of diode laser (4) interior frequency-doubling crystal, to change its microcosmic knot
Structure, and then adjust the wavelength of transmitting；
The modulation power source (3), for sending current signal to diode laser (4) according to current order；
The diode laser (4), for exporting modulation laser signal (I) according to the relationship of temperature, electric current and wavelength, frequency
To light path system (5)；
The light path system (5) is divided into two parts for that will modulate laser signal, and a part enters as reference optical signal (II)
One input port of locking phase detector (7), another part is used as detection light (III) after sample bin (6), into locking phase detector
(7) another input port；
Locking phase detector (7) for collecting reference optical signal (II) and detection light (III), and different moments absorbance is sent
To main control computer (1).
2. the super-narrow line width infrared absorption spectrum measurement device that gsec according to claim 1 is differentiated, feature exist
In the diode laser (4) transmitting central wavelength scanning range be 1-2nm, spectral line width 0.0001nm.
3. the super-narrow line width transient state infrared absorption spectrum measurement device that gsec according to claim 1 is differentiated, special
Sign is that the adjustable temperature range of the temperature control module (2) is -5 DEG C~30 DEG C.
4. the super-narrow line width transient state infrared absorption spectrum measurement device that gsec according to claim 1 is differentiated, special
Sign is that the sample bin (6) using molecular sieve tabletting sample preparation, make laser carry out multiple reflections in sample, signal is increased
Benefit.
5. the super-narrow line width transient state infrared absorption spectrum measurement device that gsec according to claim 1 is differentiated, special
Sign is that the reference optical signal (II) and detection light (III) light intensity are equal.
6. the super-narrow line width infrared absorption spectrum measurement method that gsec is differentiated, it is characterised in that the following steps are included:
(1) tabletting sample preparation after mixing sample with molecular sieve is put into sample bin (6)；
(2) main control computer (1) is by the adjusting to temperature and electric current, and to the wavelength of laser, frequency and phase are modulated, and makes
Diode laser (4) issues modulation laser signal (I)；
(3) after light path system (5), reflective portion is directly entered locking phase detector (7), becomes reference for modulation laser signal (I)
Optical signal (II)；Transmissive portion is directly entered sample bin (6), and situ catalytic reaction, the intermediary of generation occur in sample bin (6)
Kind absorbs detection light, is finally incident on locking phase detector (7), becomes detection optical signal (III)；
(4) locking phase detector (7) collects reference light (I) and detection light (III), and the absorbance of different moments is passed to master
It controls computer (1), shows time-resolved infrared absorption spectrum.
7. super-narrow line width transient state-infrared absorption spectrum measurement method that a kind of gsec according to claim 6 is differentiated,
It is characterized in that the main control computer (1) is by the adjusting to temperature and electric current, to the wavelength of laser, frequency and phase are adjusted
System the following steps are included:
It is calculated according to vibration level and the structural analysis of substance, obtains the range of the infrared absorption peak of intermediate species, and as
With reference to adjusting the output wavelength of laser；
Using the temperature of diode laser (4), electric current and wavelength, the relationship of frequency, the wavelength according to needed for sample and in advance
The frequency and phase of setting obtain corresponding temperature value, current value；
Temperature value, current value are converted into heat command respectively by main control computer (1), current order is sent to temperature control module (2) and
Modulation power source (3).
8. super-narrow line width transient state-infrared absorption spectrum measurement method that a kind of gsec according to claim 6 is differentiated,
It is characterized in that passing through formula when reference optical signal (II) and equal detection light (III) light intensityIt obtains
The absorbance of test substance, A indicate absorbance, IReference light、IDetect lightRespectively indicate reference optical signal (II) and detection light (III).
9. super-narrow line width transient state-infrared absorption spectrum measurement method that a kind of gsec according to claim 6 is differentiated,
It is characterized by: being fitted according to time-resolved infrared absorption spectrum by data, the intermediate species service life is obtained.
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