CN103529012A - Raman spectrum quantitative determination method applicable to carbon sources in blast furnace gas dust - Google Patents
Raman spectrum quantitative determination method applicable to carbon sources in blast furnace gas dust Download PDFInfo
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Abstract
The invention provides a quantitative determination method for carbon sources in blast furnace gas dust. The quantitative determination method comprises calibration and detection steps, wherein the calibration step comprises the steps: obtaining Raman spectrums of various coke samples with different coke mass ratios and determining a D peak and G peak strength ratio ID/IG according to the Raman spectrums, and a trough lowest point V peak and G peak strength ratio IV/IG between a D peak and a G peak, and taking the D peak and G peak strength ratio ID/IG and the trough lowest point V peak and G peak strength ratio IV/IG as evaluation indexes to establish a mapping relation between the ratio of carbon-containing substances in coal of the sample or a coke sample and the evaluation indexes; the detection step comprises the steps: carrying out a Raman spectrum analysis on the blast furnace gas dust to be detected and determining the ID/IG and the IV/IG; matching on the established mapping relation according to the two strengths; and determining the ratio of the carbon-containing substances of the coal or the coke of the blast furnace gas dust to be detected so as to obtain the carbon sources. According to the quantitative determination method for the carbon sources in the blast furnace gas dust, the ratio of the carbon-containing substances of the coal or the coke can be quantitatively analyzed based on the Raman spectrum analysis; the method is reliable, simple and rapid to operate, strong in applicability and low in cost.
Description
Technical field
The invention belongs to coal component fields of measurement, more specifically, relate to the quantitative detecting method of carbon source in a kind of blast furnace dust.
Background technology
In iron-making production, reducing coke use amount, increase coal powder blowing amount, is the important directions of blast furnace production sustainable development.Along with the increase of injecting coal quantity, blast-furnace tuyere region is due to the limited rough burning phenomenon that can occur in various degree coal dust in combustion space, and in blast furnace dust, carbon content can increase thereupon, and coal dust utilization ratio is restricted.Therefore, how to organize better the combustion process after pulverized coal injection, the guidance that provides for increasing Coal Injection Amount into BF and improving coal dust replacement ratio science, need to detect carbon source in blast furnace dust.
In the relevant quantitative test of coal component, people generally adopt several somes methods in petrographic analysis, simple to operate because of it, the widespread use without expensive device simultaneously.But the workload in experiment is very large, and this is a method quite consuming time, and experimental result is subject to artificial subjective factor, need professional knowledge and how to draw by rule of thumb, and being subject to the less impact of number of pictures, error is often larger.
Sreen analysis is to determine varigrained distribution in particle, but can not analyze quantitatively different carbonaceous materials in blast furnace dust and gas mud.
Ultimate analysis can draw the total carbon content in blast furnace dust, but cannot distinguish, derives from coal dust or coke.
Above method combines can determine coke and quality of pc ratio in gas ash quantitatively, and carbon content separately.But the workload of the method is quite large, practice is got up and is very required great effort, and operability is not strong, and error is often larger, and discomfort is combined into a kind of method generally adopting.
Summary of the invention
For above defect or the Improvement requirement of prior art, the object of the present invention is to provide the quantitative detecting method of carbon source in a kind of blast furnace dust based on Raman spectrum analysis, the method is reliable, simple to operate, quick, applicability is strong.
A quantitative detecting method for blast furnace dust carbon source, comprises demarcating steps and detecting step,
Described demarcating steps is: the coal tar sample that obtains in advance multiple different coal tar quality ratios, respectively to each sample surfaces projecting laser, reception, from the scattered light of sample surfaces, is carried out spectral analysis to it and is obtained Raman spectrum, according to the Raman spectrum of sample, determines that D peak and G peak intensity compare I
d/ I
g, and the peak-to-peak trough minimum point V of D peak and G compares I with G peak intensity
v/ I
g, this two intensity is compared to evaluation index, coal or the coke of setting up each sample account for the ratio of carbonaceous material in sample and the mapping relations between evaluation index;
Described detecting step is: to blast furnace gas gray surface projecting laser to be measured, receive the scattered light from blast furnace gas gray surface to be measured, it is carried out to spectral analysis and obtain Raman spectrum, according to the Raman spectrum of blast furnace dust to be measured, determine that D peak and G peak intensity compare I
d/ I
g, and the peak-to-peak trough minimum point V of D peak and G compares I with G peak intensity
v/ I
g, the mapping relations of setting up in demarcating steps according to this two strength ratio are mated, thereby determine the coal of blast furnace dust to be measured or the ratio that coke accounts for its carbonaceous material, according to this ratio, can know carbon source.
Further, also the Raman spectrum of sample and blast furnace dust to be measured has been carried out to normalized.
Further, described evaluation index also comprises that 2D peak and G peak intensity compare I
2D/ I
g.
Further, adopt the coal tar sample under different temperatures in inert atmosphere.
In general, compared with prior art, because the unconsumed pulverized coal in blast furnace dust is different with the heat treatment degree of coke process, the graphitization degree of their carbon structure is also just different for the above technical scheme of conceiving by the present invention.And Raman spectroscopy can directly be used for measuring the sample (can only be arrived by Ear Mucosa Treated by He Ne Laser Irradiation) of any size, shape, transparency, characterize C-C, C=C, the infrared weak functional group such as N=N, is that a kind of applicability is strong, measuring accuracy is high, without the Dynamic Non-Destruction Measurement of sample preparation.After adopting this Raman spectroscopy to detect gas ash sample, the structural information of its molecule can be reflected in Raman spectrogram, and the present invention selects two characteristic peaks I
d/ I
gand I
v/ I
gcharacterize the sequence degree of carbon structure.Can obtain following by the characteristic peaks I of the coal dust of known different proportion and the mixed sample of coke
d/ I
gand I
v/ I
gi with gas ash
d/ I
gand I
v/ I
grelatively, determine quantitatively the ratio of unconsumed pulverized coal in gas ash carbonaceous material, find out the principal ingredient of its carbon source.The inventive method is reliable, simple to operate, quick, usability is strong, cost is low, the coal dust utilization factor and improve coal combustion rate and reduce costs and have important directive significance to selecting coal, rationally coal powder injection, while determining different injecting coal quantity.
Accompanying drawing explanation
Fig. 1 is the original Raman spectrogram of smelter coke in the present invention;
Fig. 2 is Raman data process flow figure in the present invention;
Fig. 3 is the normalization Raman spectrogram of coke in the present invention;
Fig. 4 is the normalization Raman spectrogram of 1500 ℃ of coal tars in the present invention;
Fig. 5 is the normalization Raman spectrogram of gas ash in the present invention;
Fig. 6 is the normalization Raman spectrogram of the mixed sample of different known proportion in the present invention;
Fig. 7 is the characteristic peak normalized intensity ratio figure of the mixed sample of different known proportion in the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.In addition,, in each embodiment of described the present invention, involved technical characterictic just can not combine mutually as long as do not form each other conflict.
Raman spectroscopy is a kind of Dynamic Non-Destruction Measurement, can observe the microstructure change situation of different carbonaceous materials.The penetration depth of excitation source can reach hundreds of nanoscales, in most cases, even can obtain sample interior structural information, can also carry out macroscopic view characterize micron-sized thing.Because the diameter of laser beam is less, and can further focus on, thereby denier sample all can be measured.So Raman spectrum can solve the quantitative inaccurate problem of petrographic analysis effectively.
Raman spectrum is a scattering process, thereby the sample of any size, shape, transparency, as long as can be arrived by Ear Mucosa Treated by He Ne Laser Irradiation, just can directly be used for measuring.Raman scattering is divided into Stokes (Stokes) scattering (less than incident light frequency) and anti-Stokes (Anti-Stokes) scattering (larger than incident light frequency).General anti-Stokes line strength is less, and Stokes line strength is larger, in Raman spectrum analysis, is therefore the spectral line of main application.
Raman spectrum belongs to molecular vibration spectrum, can reflect the feature structure of molecule.Different chemical bonds has different vibrations, what Raman shift (Raman shift) reflected is the variation of vibrational energy level, be the difference of Raman diffused light and Rayleigh light frequency, so Raman shift is the characteristic parameter of molecular structure, it does not change with the change of lasing fluorescence frequency.Each material has the feature Raman spectrum of oneself, and the intensity of the number of Raman line, the size of shift value and bands of a spectrum etc. are all relevant with rotational energy level with material molecule vibration.This is the theoretical foundation that Raman spectrum can be used as molecular structure qualitative analysis.The two is directly proportional the concentration of the intensity of Raman line and incident intensity and sample molecule, and this is the theoretical foundation of Raman spectrum quantitative test.
People generally believe contains two kinds of carbon structures in texture of coal: crystal carbon (being wrapped in Turbostratic) and agraphitic carbon structure, in different coals, the ratio of crystal and agraphitic carbon is also different.Because unconsumed pulverized coal and coke are different through heat treatment degree, the sequence that causes coal dust (char) and the inner carbon structure of coke (coke) is difference also.Clearly, the structure of coke is higher than the order degree that does not consume coal.
During the carbon structure of research Coke and Char, researcher is usingd the carbon structure of graphite conventionally as reference.The molecular vibration pattern of single crystal graphite has six kinds of 2E
2g, 2B
2g, E
1u, A
2u.Two E
2gpattern is Raman active, at Raman frequency shift, is 1581cm
-1with low frequency neutron scattering feature 47cm
-1place finds.In infrared external reflection, find E
1u, A
2u, be infrared active.B
2goptically inactive.While exciting highly oriented pyrolytic graphite (highly ordered pyrolytic graphite) with the laser rays of 1064nm, except having E
2gpeak (1581cm
-1) outside, also can be at 2607cm
-1there is 2D peak (the second order characteristic peak of spectrum) in place, peak position moves and peak shape broadens to lower wave number section with the increase of carbon structure randomness.In the most orderly graphite-structure, 2D peak is the most obvious.The crystal structure of graphite hour, at 1284cm
-1and 1327cm
-1between there will be a new characteristic peak D peak (First Characteristic peak), move to high wave number with the increase of the randomness of carbon structure this peak-to-peak position.D peak is relevant with the border of graphite crystal, and its intensity depends on the density on border.When graphitic carbon structure becomes very unordered, 1610cm
-1it is corresponding to the defect carbon in graphite hexagonal ring that place there will be D ' peak, D ' peak.Normal and the E in this peak
2gpeak is (by E
2gpeak is grouped into the SP of hexagon graphite plane
2hydridization carbon structure) crosslinked, overlapping, form so-called G peak.1581cm
-1the G peak that place occurs is the topmost characteristic peak of graphite.At this moment 2D peak is to 2567cm
-1move and even can disappear along with the increase of randomness.
For orderly material with carbon element, such as HOPG, its Raman spectral peaks is strong, steep.But disordered carbon material, agraphitic carbon is SP
3sP in hydridization carbon and graphite
2the non-structure potpourri of hydridization carbon, its G peak and D peak-to-peak be wide wants wide many.The same with graphitic carbon, D peak is with respect to the ratio (I of G peak intensity
d/ I
g) be also measuring of agraphitic carbon disorder and order degree.I
d/ I
gvalue increases the basic graphite unit or the crystal structure that represent in Coal and coke and becomes large, I
v/ I
gminimizing and whole carbon structure that value reduces expression agraphitic carbon structure become more even.There is at present people when the Raman collection of illustrative plates of research coal tar, at 1590cm
-1and 1350cm
-1find respectively G peak and D peak.
For very orderly carbonaceous material, as graphite and HOPG, even if background signal is very weak, what their Raman peaks was suitable obviously endures with point.After baseline calibration, can assess carbon structure with acquired spectrum.With Raman spectroscopy, study graphite and other disordered carbon structures first, and point out I
d/ I
glattice dimensions (lateral dimension L in value and face
a) be negative correlativing relation.But along with the structural disorder of carbonaceous material increases, the wider and bad identification that becomes of their Raman peaks.Due to thermal effect and epipolic appearance, baseline increases significantly.
About the Raman spectrum assessment method of agraphitic carbon structure, have a variety of, generally use original (processing through deconvolution) D peak with G peak intensity than (I
d/ I
g), the half width ratio at D peak and G peak, the peak-to-peak trough minimum point V of D peak and G with G peak intensity than (I
v/ I
g) etc. parameter as the index of evaluation disordered carbon structure.G peak refers to and E
2gcorresponding first peak of mode of vibration, its formation and SP
2the vibration of the carbon atom of hydridization is relevant, is the sign that hydridization forms graphite.D peak refers to disordering peak, is that surperficial disordered carbon structure causes, and can observe the D peak that single phonon produces while there is defect.V peak refers to G peak and the peak-to-peak trough of D, is by the G between them
rpeak (on the right, G peak), V
lpeak (on the left side, V peak), V
rthe common matching in peak (on the right, V peak) forms, and these three peaks mainly represent the stretching vibration pattern in aromatic cycle compound, have two benzene ring structures in this aromatic cycle compound at least.In the present invention, original I will be used
d/ I
gand I
v/ I
gvalue is the method containing carbon structure as assessment, if further improve accuracy, also can increase I
2D/ I
gas evaluation index.2D peak is biphonon resonance raman peak, represents second order Raman graphite peaks.When irradiating highly oriented pyrolytic graphite with 1064nm exciting light, will be at 2607cm
-1there is 2D peak in displacement place.When carbon structure becomes unordered, 2D peak broadens and toward the movement of lower wave number section, even may disappear.Therefore, along with the rising of temperature, the carbon structure in coal is more orderly, 2D peak and G peak intensity ratio I
2D/ I
galso just larger.
Based on above-mentioned analysis, technical scheme of the present invention is:
First demarcate, obtain in advance the coal tar sample of multiple different coal tar quality ratios, respectively to each sample surfaces projecting laser, receive the scattered light from sample surfaces, it is carried out to spectral analysis and obtain Raman spectrum, according to the Raman spectrum of sample, determine that D peak and G peak intensity compare I
d/ I
g, and the peak-to-peak trough minimum point V of D peak and G compares I with G peak intensity
v/ I
g, this two intensity is compared to evaluation index, coal or the coke of setting up each sample account for the ratio of carbonaceous material in sample and the mapping relations between evaluation index;
Then detect, to blast furnace gas gray surface projecting laser to be measured, receive the scattered light from blast furnace gas gray surface to be measured, it is carried out to spectral analysis and obtain Raman spectrum, according to the Raman spectrum of blast furnace dust to be measured, determine that D peak and G peak intensity compare I
d/ I
g, and the peak-to-peak trough minimum point V of D peak and G compares I with G peak intensity
v/ I
g, the mapping relations of setting up in demarcating steps according to this two strength ratio are mated, thereby determine the coal of blast furnace dust to be measured or the ratio that coke accounts for its carbonaceous material.
In demarcating steps, preferably produce the sample under different condition, comprise in inert atmosphere under different high temperature through heat treated coal tar and coke.For the carbon structure difference performance of these samples is reflected in Fourier transform-Raman spectroscopy like this.Original Raman spectrum data baseline wander, burr is more, this is because be subject to surrounding environment fluorescence, the factors such as the noise of instrument self are disturbed, true sequence that cannot actual response sample carbon structure, therefore utilizes origin software to carry out respective handling to figure, by after the level and smooth normalized of these different carbonaceous materials, also the true Raman collection of illustrative plates of raw sample, carries out identification marking.
The I of the mixed sample of known proportion will be organized more
d/ I
g, I
v/ I
g, I
2Di
gvariation tendency, does Raman spectrum analysis with gas ash sample and obtains the I in spectrogram
d/ I
g, I
v/ I
g, I
2Di
gvalue contrast, determines carbon structure variation situation, can substantially draw char content or coke content in gas ash.
1) coal sample of fetching and coke sample are milled to 150-202um particle size range, after the pulverized coal sample of milled is dry, be laid in corundum porcelain boat, and be placed in tubular furnace, pass into nitrogen and form inert atmosphere, then start the heating process that heats up, produce under different high temperature through heat treated coal tar and coke.Do is like this that carbon structure difference performance by different condition sample reflects better in Fourier transform-Raman spectroscopy.Due at different heat treatment temperature, various durations does not have any difference to last sample spectra.The thermal treatment that continues 30min is complete to the carbon structure effect of carbonaceous material, the longer heat time on carbon structure without any impact.Present technique heat treatment process is with certain heating rate, to rise to 800～2000 ℃ of temperature range intervals in heating furnace, after insulation 30min, begins to cool down to 200 ℃.
Burnt sample mixes coal tar Char and coke Coke in different coal tar ratios after prepare in mortar, and the mixing of Coke+Char that obtains being mixed with different proportion Char is burnt, and numbering is as shown in table 1 afterwards.
Table 1
2) Raman spectrum test is not high to sample requirement, and it is convenient to measure, fast.In test, the thermal effect of bringing in order to eliminate better fluorescence and laser, the ratio according to the form below adds the KBr particle of some mg in sample.The above-mentioned sample making is carried out to Raman test, and the test condition of Raman is as shown in table 2.
Table 2
3) the original Raman of coke recording as shown in Figure 1, even if adding KBr particle to eliminate fluorescence in sample disturbs, but still there is baseline wander in this Raman collection of illustrative plates, single order and second-order Raman scattering band are wider, and whole curve is with many spines, several characteristic peaks are more not obvious, also reflect and in coke, have very unordered carbon structure.Generally, the spectrum of experiment gained mainly consists of three compositions: from the spectrum of sample, from the disturbance spectrum of environment and the background spectra of measure spectrum instrument generation itself.From the spectrum of sample, generally also can comprise and place the noise spectrum that rebasing, the container of test substance or solution etc. produce.The disturbance spectrum of environment mainly comprises the disturbance spectrum causing from cosmic rays, special experiment condition, environment and environmental change etc.: from the ground unrest spectrum of spectral instrument, mainly comprise the intrinsic noise of instrument itself, and the noise spectrum of the improper generation of adjusting of instrument.
In sum, because measured original spectrum is " non-real spectrum ", can not directly obtain the characteristic peaks (being G peak and D peak) of sample carbon structure.The present invention utilizes origin software to take corresponding means to process Raman data, goes back the true collection of illustrative plates of raw sample, and its treatment scheme as shown in Figure 2.First utilize smoothing method to eliminate and reduce noise spectrum, selecting " FFT Filter " in origin, " Points of windows " is set to 20, and curve is become to level and smooth.Secondly the correction to the baseline wander of collection of illustrative plates, suitably improves by the method for fitting of a polynomial, the interference of deduction fluorescence or other " impurity spectrums ".In origin, select " Peak Analyzer ", according to curve tendency figure, select voluntarily some baseline points near finding ，Gai position, characteristic peak position.Because the degree of correlation of the Raman curve with at the bottom of lienar for baseline button and primary curve is the highest, so baseline type is " interpolation method " selection lienar in software.Finally, by curve normalized, eliminate some disturbing influences.Here use in collection of illustrative plates and compose strong peak (being D peak) as the quantitative analysis method of normalization reference.In origin, select " Normalize Columns ", be set to " divided by max ".Normalized formula is as follows
Wherein, s
ifor each spectrum point intensity in former spectrum, s is reference point, s
i' be the value after normalization.
4) the original Raman data of institute's test sample product is processed as stated above, obtained the normalization Raman collection of illustrative plates of the mixed sample of smelter coke, 1500 ℃ of coal tar samples, gas ash and five groups of known component ratios, as shown in Fig. 3-Fig. 7.Arrange again each sample chromatogram characteristic peak intensity, and draw the strength ratio after normalization, as shown in table 3.
Table 3
| Sample | Char?ratio | I G/I D | I 2D/I D | I V/I D |
| Metallurgical?Coke | 0 | 0.6813 | 0.2193 | 0.3975 |
| 1500℃Char | 100 | 0.5703 | 0.7415 | 0.1145 |
| 10%Char | 10 | 0.5879 | 0.3465 | 0.2336 |
| 20%Char | 20 | 0.8143 | 0.4673 | 0.2044 |
| 30%Char | 30 | 0.6179 | 0.2533 | 0.3146 |
| 40%Char | 40 | 0.6594 | 0.4245 | 0.2924 |
| 50%Char | 50 | 0.6082 | 0.3268 | 0.2435 |
| Dust | ? | 0.5859 | 0.3463 | 0.2361 |
5) the characteristic peak normalized intensity ratio of the mixed sample of different proportion in table 4 is plotted to curve map, as shown in Figure 7.
The object of the invention is to different carbonaceous materials distinguish and and sample in the quantitative test of certain carbonaceous material, its method is that the Raman collection of illustrative plates of the Raman collection of illustrative plates of blast furnace dust to be measured and five groups of known proportion samples is analyzed relatively, the order degree of considering different material carbon structure is different, can effectively to different carbonaceous materials, carry out identification marking, determine carbon structure variation situation.Then according to the I of the mixed sample of Fig. 7 known proportion
d/ I
g, I
v/ I
g, I
2D/ I
gvariation tendency, does Raman spectrum analysis with gas ash sample and obtains the I in spectrogram
d/ I
g, I
v/ I
g, I
2D/ I
gvalue contrast, can show that the char content in gas ash is 10%, and the ratio that the unconsumed pulverized coal that shows certain blast furnace dust only accounts for carbonaceous material is 10% left and right, the most of source of carbonaceous material coke in ash.The combustion case of this test findings explanation coal injection at blast-furnace tuyere place is good, and its utilization factor is higher; In order to reduce this blast furnace dust carbon content, must improve the quality of coke.
In above-described embodiment, using char content as the explanation of quantitative test physics amount example, also can as quantitative test physics amount, carry out similar analysis by Coke content.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. a quantitative detecting method for blast furnace dust carbon source, comprises demarcating steps and detecting step, it is characterized in that,
Described demarcating steps is: the coal tar sample that obtains in advance multiple different coal tar quality ratios, respectively to each sample surfaces projecting laser, reception, from the scattered light of sample surfaces, is carried out spectral analysis to it and is obtained Raman spectrum, according to the Raman spectrum of sample, determines that D peak and G peak intensity compare I
d/ I
g, and the peak-to-peak trough minimum point V of D peak and G compares I with G peak intensity
v/ I
g, this two intensity is compared to evaluation index, coal or the coke of setting up each sample account for the ratio of carbonaceous material in sample and the mapping relations between evaluation index;
Described detecting step is: to blast furnace gas gray surface projecting laser to be measured, receive the scattered light from blast furnace gas gray surface to be measured, it is carried out to spectral analysis and obtain Raman spectrum, according to the Raman spectrum of blast furnace dust to be measured, determine that D peak and G peak intensity compare I
d/ I
g, and the peak-to-peak trough minimum point V of D peak and G compares I with G peak intensity
v/ I
g, the mapping relations of setting up in demarcating steps according to this two strength ratio are mated, thereby determine the coal of blast furnace dust to be measured or the ratio that coke accounts for its carbonaceous material, according to this ratio, can know carbon source.
2. the quantitative detecting method of blast furnace dust carbon source as claimed in claim 1, is characterized in that, also the Raman spectrum of sample and blast furnace dust to be measured has been carried out to normalized.
3. the quantitative detecting method of blast furnace dust carbon source as claimed in claim 1 or 2, is characterized in that, described evaluation index also comprises that 2D peak and G peak intensity compare I
2D/ I
g.
4. the quantitative detecting method of blast furnace dust carbon source as claimed in claim 1 or 2, is characterized in that, adopts the coal tar sample under different temperatures in inert atmosphere.
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