CN103529012B - A kind of Raman spectrum quantitative being applicable to carbon source in blast furnace dust - Google Patents
A kind of Raman spectrum quantitative being applicable to carbon source in blast furnace dust Download PDFInfo
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Abstract
The invention provides a kind of quantitative detecting method of blast furnace dust carbon source, comprise demarcation and detecting step; Demarcating steps is: the Raman spectrum obtaining the coal tar sample of multiple different coal tar quality ratio, determines that D peak compares I with G peak intensity according to Raman spectrum
d/ I
g, and the D peak trough minimum point V peak-to-peak with G compares I with G peak intensity
v/ I
g, it can be used as evaluation index, set up the coal of sample or coke and account for mapping relations between the ratio of carbonaceous material in sample and evaluation index; Detecting step is: to the Raman spectrum analysis of blast furnace dust to be measured, determine I
d/ I
gand I
v/ I
g, mate according to the mapping relations that this two strength ratio is being set up, determine that the coal of blast furnace dust to be measured or coke account for the ratio of its carbonaceous material, and then know carbon source.The present invention is based on Raman spectrum analysis and analyze the ratio that coal or coke account for its carbonaceous material quantitatively, the method is reliable, simple to operate, quick, usability is strong, cost is low.
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 fumance sustainable development.Along with the increase of injecting coal quantity, the rough burning phenomenon that blast-furnace tuyere region can occur coal dust in various degree because combustion space is limited, in blast furnace dust, carbon content can increase thereupon, and coal dust utilization ratio is restricted.Therefore, how to organize the combustion process after pulverized coal injection better, provide guidance for what increase Coal Injection Amount into BF and improve coal dust replacement ratio science, need to detect carbon source in blast furnace dust.
In the quantitative test that coal component is relevant, people generally adopt several somes methods in petrographic analysis, because it is simple to operate, and the widespread use without the need to 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, and 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.
Varigrained distribution in particle is determined in sreen analysis, but can not analyze different carbonaceous material in blast furnace dust and gas mud quantitatively.
Ultimate analysis can draw the total carbon content in blast furnace dust, but cannot distinguish and derive from coal dust or coke.
Above methods combining gets up to determine quantitatively coke and quality of pc ratio in gas ash, and respective carbon content.But the workload of the method is quite large, practice gets up extremely to require great effort, and operability is not strong, and error is often comparatively large, and discomfort is combined into a kind of method generally adopted.
Summary of the invention
For above defect or the Improvement requirement of prior art, the object of the present invention is to provide a kind of quantitative detecting method based on carbon source in the blast furnace dust of 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 obtaining multiple different coal tar quality ratio in advance, respectively to each sample surface projecting laser, receive the scattered light from sample surfaces, carry out spectral analysis obtain Raman spectrum to it, the Raman spectrum according to sample determines that D peak compares I with G peak intensity
d/ I
g, and the D peak trough minimum point V peak-to-peak with G compares I with G peak intensity
v/ I
g, using this two intensity than as evaluation index, set up the coal of each sample or coke and account for mapping relations between the ratio of carbonaceous material in sample and 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, carry out spectral analysis obtain Raman spectrum to it, the Raman spectrum according to blast furnace dust to be measured determines that D peak compares I with G peak intensity
d/ I
g, and the D peak trough minimum point V peak-to-peak with G compares I with G peak intensity
v/ I
g, the mapping relations set up in demarcating steps according to this two strength ratio are mated, thus determine that the coal of blast furnace dust to be measured or coke account for the ratio of its carbonaceous material, can know carbon source according to this ratio.
Further, also normalized has been carried out to the Raman spectrum of sample and blast furnace dust to be measured.
Further, described evaluation index also comprises 2D peak and compares I with G peak intensity
2D/ I
g.
Further, the coal tar sample under different temperatures is in an inert atmosphere adopted.
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 conceived by the present invention.And Raman spectroscopy directly can be used for measuring the sample (can only be irradiated with a laser) of any size, shape, transparency, characterize C-C, the infrared more weak functional group such as C=C, N=N, is that a kind of applicability is strong, measuring accuracy is high, without the need to 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.The following characteristic peaks I coal dust of known different proportion and coke being mixed sample can be obtained
d/ I
gand I
v/ I
gwith the I of gas ash
d/ I
gand I
v/ I
grelatively, determine the ratio of unconsumed pulverized coal in gas ash carbonaceous material quantitatively, find out the principal ingredient of its carbon source.The inventive method is reliable, simple to operate, quick, usability is strong, cost is low, to selection coal, rationally coal powder injection, determine different injecting coal quantity time coal utilization and improve coal combustion rate and reduce costs there is important directive significance.
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 DEG C 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 that in the present invention, different known proportion mixes sample;
Fig. 7 is the characteristic peak normalized intensity ratio figure that in the present invention, different known proportion mixes sample.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, 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, be not intended to limit the present invention.In addition, if below in described each embodiment of the present invention involved technical characteristic do not form conflict each other and just can mutually combine.
Raman spectroscopy is a kind of Dynamic Non-Destruction Measurement, can observe the microstructure change situation of different carbonaceous material.The penetration depth of excitation source can reach hundreds of nanoscale, in most cases, even can obtain sample interior structural information, can also carry out macroscopic token to micron-sized thing.Because the diameter of laser beam is less, and can focus on further, thus 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, the thus sample of any size, shape, transparency, as long as can be irradiated with a laser, just can directly be used for measuring.Raman scattering is divided into Stokes (Stokes) scattering (less than the frequency of incident light) and anti-Stokes (Anti-Stokes) scattering (larger than the frequency of incident light).General anti-Stokes line strength is less, and Stokes line strength is comparatively large, is therefore the spectral line of main application in Raman spectrum analysis.
Raman spectrum belongs to molecular vibration spectrum, can reflect the feature structure of molecule.Different chemical bonds has different vibrations, the change of vibrational energy level that what Raman shift (Ramanshift) reflected is, be the difference of the frequency of Raman diffused light and Reyleith scanttering light, therefore Raman shift is the characteristic parameter of molecular structure, and it does not change with the change of lasing fluorescence frequency.Each material has oneself Raman spectrum, and the intensity etc. of the number of Raman line, the size of shift value and bands of a spectrum is all vibrated relevant with rotational energy level with material molecule.This is that Raman spectrum can as the theoretical foundation of molecular structure qualitative analysis.The intensity of Raman line is directly proportional to both the concentration of 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 amorphous carbon structure, in different coals, the ratio of crystal and agraphitic carbon is also different.Due to unconsumed pulverized coal and coke different through heat treatment degree, cause the sequence of coal dust (char) and coke (coke) inner carbon structure also different.Clearly, not consume the order degree of coal higher for the structural rate of coke.
When studying the carbon structure of Coke and Char, researcher is usually using the carbon structure of graphite 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, is 1581cm at Raman frequency shift
-1with low frequency neutron scattering feature 47cm
-1place finds.E is found in infrared external reflection
1u, A
2u, be infrared active.B
2goptically inactive.When exciting highly oriented pyrolytic graphite (highlyorderedpyrolyticgraphite) with the laser rays of 1064nm, except having E
2gpeak (1581cm
-1) outward, also can at 2607cm
-1there is 2D peak (the second order characteristic peak of spectrum) in place, peak position to move 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.When the crystal structure of graphite is less, at 1284cm
-1and 1327cm
-1between there will be a new characteristic peak D peak (fisrt feature peak), this peak-to-peak position is moved to high wave number with the increase of the randomness of carbon structure.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
-1place there will be D ' peak, and D ' peak corresponds to the defect carbon in graphite hexagonal ring.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, suddenly.But disordered carbon material, agraphitic carbon is SP
3sP in hydridization carbon and graphite
2the non-structural potpourri of hydridization carbon, its G peak and D peak-to-peak wide want wide many.The same with graphitic carbon, D peak is relative to the ratio (I of G peak intensity
d/ I
g) be also measuring of agraphitic carbon disorder and order degree.I
d/ I
gbasic graphite unit in value increase expression Coal and coke or crystal structure become large, I
v/ I
gvalue minimizing represents that the minimizing of amorphous carbon structure and whole carbon structure become more even.There is people at present when studying the Raman collection of illustrative plates of coal tar, at 1590cm
-1and 1350cm
-1find G peak and D peak respectively.
For very orderly carbonaceous material, as graphite and HOPG, even if background signal is very weak, their suitable obviously the enduring with point of Raman peaks.After baseline calibration, carbon structure can be assessed with acquired spectrum.First by Raman spectroscopy research graphite and other disordered carbon structures, and point out I
d/ I
gvalue and lattice dimensions (the lateral dimension L in face
a) in negative correlativing relation.But along with the structural disorder of carbonaceous material increases, their Raman peaks become wider and bad identification.Due to thermal effect and epipolic appearance, baseline increases significantly.
Raman spectrum assessment method about amorphous carbon structure has a variety of, general use original (not through deconvolution process) D peak and G peak intensity ratio (I
d/ I
g), the half width ratio at D peak and G peak, the trough minimum point V that D peak is peak-to-peak with G and G peak intensity ratio (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 mark that hydridization forms graphite.D peak refers to disordering peak, is that interface disorder carbon structure causes, and can observe the D peak that single phonon produces during existing defects.V peak refers to G peak and the peak-to-peak trough of D, is by the G between them
rpeak (on the right of G peak), V
lpeak (on the left side, V peak), V
rthe common matching in peak (on the right of V peak) is formed, 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
gbe worth as the method for assessment containing carbon structure, if improve accuracy further, 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 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 larger.
Based on above-mentioned analysis, technical scheme of the present invention is:
First demarcate, obtain the coal tar sample of multiple different coal tar quality ratio in advance, respectively to each sample surface projecting laser, receive the scattered light from sample surfaces, carry out spectral analysis to it and obtain Raman spectrum, the Raman spectrum according to sample determines that D peak compares I with G peak intensity
d/ I
g, and the D peak trough minimum point V peak-to-peak with G compares I with G peak intensity
v/ I
g, using this two intensity than as evaluation index, set up the coal of each sample or coke and account for mapping relations between the ratio of carbonaceous material in sample and 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, carry out spectral analysis obtain Raman spectrum to it, the Raman spectrum according to blast furnace dust to be measured determines that D peak compares I with G peak intensity
d/ I
g, and the D peak trough minimum point V peak-to-peak with G compares I with G peak intensity
v/ I
g, the mapping relations set up in demarcating steps according to this two strength ratio are mated, thus determine that the coal of blast furnace dust to be measured or coke account for the ratio of its carbonaceous material.
In demarcating steps, preferably produce the sample under different condition, to comprise in inert atmosphere under different high temperature through heat treated coal tar and coke.In order to 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 factor interference such as the noise of instrument self, cannot the true sequence of actual response sample carbon structure, therefore utilize origin software to carry out respective handling to figure, 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.
To known proportion be organized more mix the I of sample
d/ I
g, I
v/ I
g, I
2Di
gvariation tendency, is with gas ash sample the I that Raman spectrum analysis obtains in spectrogram
d/ I
g, I
v/ I
g, I
2Di
gvalue contrast, determines carbon structure variation situation, substantially can draw the char content in gas ash or coke content.
Embodiment 1
1) coal sample fetched and coke sample are milled to 150-202um particle size range, be laid in corundum porcelain boat by after the pulverized coal sample drying of milled, 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 like this is 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.Namely the thermal treatment continuing 30min is complete to the carbon structure effect of carbonaceous material, the longer heat time on carbon structure without any impact.This technomania processing procedure rises to 800 ~ 2000 DEG C of temperature range intervals with certain heating rate in heating furnace, begins to cool down to 200 DEG C after insulation 30min.
Burnt sample mixes coal tar Char and coke Coke in different coal tar ratios after having prepared in mortar, and the mixing obtaining the Coke+Char being mixed with different proportion Char is burnt, as shown in table 1 after numbering.
Table 1
2) Raman spectrum test is not high to sample requirement, and it is convenient to measure, fast.In testing, in order to eliminate the thermal effect that fluorescence and laser bring better, the ratio according to the form below adds the KBr particle of some mg in sample.The above-mentioned sample made is carried out Raman test, and the test condition of Raman is then as shown in table 2.
Table 2
3) the original Raman of the coke recorded as shown in Figure 1, even if add KBr particle in the sample to eliminate fluorescence interference, but still there is baseline wander in this Raman collection of illustrative plates, single order and second-order Raman scattering band wider, and whole curve is with many spines, several characteristic peak is more not obvious, also reflects there is very unordered carbon structure in coke.Generally, the spectrum of testing gained is formed primarily of three compositions: the own reasons for its use spectrum of the spectrum from sample, the disturbance spectrum from environment and measure spectrum instrument.Spectrum from sample generally also can comprise the noise spectrum that rebasing, the container of placing test substance or solution etc. produce.The disturbance spectrum of environment mainly comprises the disturbance spectrum caused from cosmic rays, special experiment condition, environment and environmental change etc.: the ground unrest spectrum from spectral instrument mainly comprises the intrinsic noise of instrument itself, and the noise spectrum of the improper generation of the adjustment of instrument.
In sum, because measured original spectrum is " non-genuine spectrum ", the characteristic peaks (i.e. G peak and D peak) of sample carbon structure directly can not be obtained.The present invention utilizes origin software to take corresponding means to process Raman data, and go back the true collection of illustrative plates of raw sample, its treatment scheme as shown in Figure 2.First utilize smoothing method to eliminate and reduce noise spectrum, in origin, select " FFTFilter ", " Pointsofwindows " is set to 20, and curve is become level and smooth.Secondly the correction to the baseline wander of collection of illustrative plates, namely suitably improves by the method for fitting of a polynomial, the interference of deduction fluorescence or other " impurity spectrums ".In origin, select " PeakAnalyzer ", according to curve tendency figure, find characteristic peak position, near this position, select some baseline points voluntarily.Due to the highest by the degree of correlation of the Raman curve at the bottom of lienar for baseline button and primary curve, " interpolationmethod " select linear type therefore in baseline type and software.Finally by curve normalized, eliminate some disturbing influences.Here use in collection of illustrative plates and compose the quantitative analysis method of strong peak (i.e. D peak) as normalization reference.In origin, select " NormalizeColumns ", be set to " dividedbymax ".Normalized formula is as follows
Wherein, s
ifor spectrum point intensity each 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, obtain the normalization Raman collection of illustrative plates of mixed sample of smelter coke, 1500 DEG C of coal tar samples, gas ash and five groups of known component ratios, as shown in Fig. 3-Fig. 7.Arrange each sample chromatogram characteristic peak intensity again, 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) characteristic peak normalized intensity ratio different proportion in table 4 being mixed sample plots curve map, as shown in Figure 7.
The object of the invention is to distinguish different carbonaceous material and and sample in the quantitative test of certain carbonaceous material, its method is that the Raman collection of illustrative plates of blast furnace dust to be measured and the Raman collection of illustrative plates of five groups of known proportion samples are carried out com-parison and analysis, consider that the order degree of different material carbon structure is different, effectively can carry out identification marking to different carbonaceous materials, determine carbon structure variation situation.Then the I of sample is mixed according to Fig. 7 known proportion
d/ I
g, I
v/ I
g, I
2D/ I
gvariation tendency, is with gas ash sample the I that Raman spectrum analysis obtains 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%, shows that the ratio that the unconsumed pulverized coal of certain blast furnace dust only accounts for carbonaceous material is about 10%, carbonaceous material major part source coke in ash.This test findings illustrates that coal injection is good at the combustion case at blast-furnace tuyere place, and its utilization factor is higher; In order to reduce this blast furnace dust carbon content, the quality of coke must be improved.
In above-described embodiment, illustrate using char content as quantitative test physics amount example, also can carry out similar analysis as quantitative test physics amount 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 amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (3)
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 obtaining multiple different coal tar quality ratio in advance, respectively to each sample surface projecting laser, receive the scattered light from sample surfaces, carry out spectral analysis obtain Raman spectrum to it, the Raman spectrum according to sample determines that D peak compares I with G peak intensity
d/ I
g, and the D peak trough minimum point V peak-to-peak with G compares I with G peak intensity
v/ I
g, using this two intensity than as evaluation index, set up the coal of each sample or coke and account for mapping relations between the ratio of carbonaceous material in sample and 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, carry out spectral analysis obtain Raman spectrum to it, the Raman spectrum according to blast furnace dust to be measured determines that D peak compares I with G peak intensity
d/ I
g, and the D peak trough minimum point V peak-to-peak with G compares I with G peak intensity
v/ I
g, the mapping relations set up in demarcating steps according to this two strength ratio are mated, thus determine that the coal of blast furnace dust to be measured or coke account for the ratio of its carbonaceous material, can know carbon source according to this ratio.
2. the quantitative detecting method of blast furnace dust carbon source as claimed in claim 1, is characterized in that, also carried out normalized to the Raman spectrum of sample and blast furnace dust to be measured.
3. the quantitative detecting method of blast furnace dust carbon source as claimed in claim 1 or 2, it is characterized in that, described evaluation index also comprises 2D peak and compares I with G peak intensity
2D/ I
g.
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| 不同变质程度煤的激光拉曼光谱特征;段菁春;《地质科技情报》;20020630;第21卷(第2期);第65-68页 * |
| 不同煤级煤的Raman谱特征及与XRD结构参数的关系;李美芬 等;《光谱学与光谱分析》;20090930;第29卷(第9期);第2446-2449页 * |
| 高炉炉尘中未消耗煤粉和焦炭比例的研究;郑涛 等;《钢铁》;20030331;第41卷(第3期);第20-24页 * |
| 高炉瓦斯灰中未燃煤粉和焦炭比例的研究与实践;尹坚;《炼铁技术通讯》;20091231(第1期);第22-24页 * |
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