CN104198514A - Method for identifying properties of manganese ore and manganese smelting slag - Google Patents
Method for identifying properties of manganese ore and manganese smelting slag Download PDFInfo
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- CN104198514A CN104198514A CN201410485052.2A CN201410485052A CN104198514A CN 104198514 A CN104198514 A CN 104198514A CN 201410485052 A CN201410485052 A CN 201410485052A CN 104198514 A CN104198514 A CN 104198514A
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Abstract
The invention relates to a method for identifying properties of manganese ore and manganese smelting slag. According to the method, the properties of the manganese ore and the manganese smelting slag are identified by an X-ray diffraction spectroscopic method and an infrared spectroscopic method, characteristic spectral peaks of soft manganese ore, manganese oxide, manganosite, rhodochrosite and the like in the manganese ore are found by X-ray diffraction spectra, and the spectral peaks of the soft manganese ore, the manganese oxide, the manganosite, the rhodochrosite and the like in the manganese ore are analyzed and compared with characteristic peaks of iron silicate and the like of the manganese smelting slag for identifying the properties of the manganese ore; at the same time, corroborating is performed by infrared spectral characteristics, in the range of 600-400 cm<-1>, the manganese ore has two strong absorption bands, and individually or simultaneously has characteristic absorption peaks at 1420 cm<-1>, and the manganese smelting slag has a wide strong absorption peak at about 960 cm<-1>. By the method, the properties of the manganese ore can be confirmed and identified at the same time; the method can provide technical support for inspection and quarantine and Customs and can provide a scientific identification report for traders, so that border security is ensured and environment pollution and trading fraud are avoided.
Description
Technical field
The present invention relates to the discrimination method of manganese ore, particularly a kind of manganese ore and manganese metallurgical slag attribute discrimination method,
This method is applicable to inspection and quarantine system, customs, R&D institution, universities and colleges, inspection center and manufacturer manganese ore and manganese metallurgical slag attribute is differentiated.
Background technology
Manganese ore refers to the manganese-bearing mineral that natural conditions form, the purposes that is mainly used in refining manganese.In modern industry, manganese and compound thereof are applied to the every field of national economy, and wherein steel and iron industry is most important field, account for 90%～95% by manganese amount, mainly as deoxidizer and desulfurizing agent in ironmaking and steelmaking process, and are used for alloying.China has listed manganese in the Eleventh Five-Year Plan period national strategy resource, and visible manganese ore has very important strategic position.Therefore the foreign trade that, increasing enterprise, company have carried out manganese ore.
Under market, cause unordered competition, pursue maximum profit, cause domestic and international illegal retailer to adulterate, pass a fake product off as a genuine one, the phenomenon of the melting waste slag of doping China import prohibition constantly occurs, has had a strong impact on the trading enviroment of China, damage the interests of importer, the ecologic environment of China has been caused to havoc simultaneously.Manganese mud is taking the oxide of silicon, calcium as main, and manganese content is lower, smelt be worth very low, and contain a large amount of poisonous and harmful heavy metallics, as lead, zinc, arsenic, copper, above-mentioned harmful heavy metal meeting polluted surface water, underground water and soil, do great damage to ecologic environment.
And formed and content by similar element to some manganese ores due to manganese metallurgical slag, list sometimes cannot be accurately by its difference from the height of constituent content.China does not still have effective manganese ore and manganese metallurgical slag discrimination method at present, the departments such as customs is investigated and prosecuted and cause considerable trouble, so urgently set up effective discrimination method of manganese ore and metallurgical slag thereof, better safeguards national economic interest, protects national ecologic environment.
Summary of the invention
Object of the present invention is exactly for overcoming the deficiencies in the prior art, differentiate a difficult problem for manganese ore and manganese metallurgical slag, a kind of effectively discrimination method is provided, go through several years, collect by the relevant attribute of manganese ore, manganese metallurgical slag being differentiated to mass data, and the data of collection is sorted out, after Comparative Study, finally successfully find out the attribute discrimination method of a kind of manganese ore and manganese metallurgical slag; Simultaneously, taking this method can serve department etc. between inspection and quarantine, customs, R&D institution, universities and colleges, inspection center and corresponding manufacturer differentiates the classification of the mineral waste and old material of import class, stop industrial refuse immigration by technological means, ensured China's Environmental security.
The present invention realizes by such technical scheme: a kind of discrimination method that manganese ore and manganese metallurgical slag are distinguished, is characterized in that: taken separately discriminating step is as follows:
(1), draw samples quantity is no less than 100g, by the sample splitting of extraction, be crushed to all by 200 eye mesh screens;
(2), adopt pressed disc method, adopt X-fluorescence spectrometer to carry out sxemiquantitative scanning to sample, whether preliminary judgement sample belongs to the scope of manganese ore and manganese metallurgical slag, if do not belong to the scope of manganese ore and manganese metallurgical slag, do not belong to the discriminating scope of this method, if belong to the scope of manganese ore and manganese metallurgical slag, carry out again the analysis of next step;
(3), take X-ray diffraction spectroscopic methodology to carry out X-ray diffraction spectral analysis to sample;
A) sample being placed in to the temperature with 105 DEG C in drying baker dries, then the sample after drying is put into sample box, after compacting, put into X-ray diffraction spectrometer sample chamber, scan and deposit scan-data in spectrogram storehouse through X-ray diffraction spectrometer, by X-ray diffraction spectrometer automatic analysis spectrum peak, obtain a result, data storing is to be checked;
If b) X-ray diffraction spectral analysis result exists obvious manganese metallurgical slag characteristic spectrum peak, judgement sample attribute is manganese metallurgical slag, but not manganese ore, otherwise need to carry out next step;
(4), adopt fourier transform infrared spectroscopy to carry out characteristic infrared absorption spectrum analysis to the sample after step (3) inspection:
A) require preparation to detect sample according to infrared spectrum sample, sample is placed into and in spectrum chamber, detects and to record spectrogram to be checked;
If b) the results of FT-IR exists obvious manganese metallurgical slag characteristic, judgement sample attribute is manganese metallurgical slag, otherwise can judge that this sample is manganese ore.
The beneficial effect that the present invention produces is:
Manganese ore is clearly proposed and manganese metallurgical slag is compared authentication technique.Taking technical measures as means, taking Supervision Measures as target, this authentication method has reached to be blocked imported goods and renames the object of making a breakthrough from source, for inspection and quarantine, customs provide technical support, for trade people provides the probation report of science, guarantee border safety, avoid environmental pollution.
Brief description of the drawings
Fig. 1 is manganese ore X-ray diffraction spectrogram;
Fig. 2 is manganese metallurgical slag X-ray diffraction spectrogram;
Fig. 3 is manganese ore infrared spectrogram;
Fig. 4 is manganese metallurgical slag (the cooling slag of air) infrared spectrogram;
Fig. 5 is the infrared signature spectrogram of rhodochrosite;
Fig. 6 is the infrared signature spectrogram of manganese metallurgical slag (Water Quenching Slag);
The infrared signature spectrogram of Fig. 7 manganese metallurgical slag (rich manganese slag).
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
The present invention's research work in early stage mainly comprises the following aspects:
1, research manganese ore and manganese metallurgical slag otherness
Comprehensive collection, arrange the classification of domestic and international manganese ore, manganese metallurgical slag, specification, understand manganese ore production and processing technology, specify which kind of production technology and will produce which kind of manganese metallurgical slag, thereby find out both essence difference, clearly differentiate directivity target.
2, research manganese ore and manganese metallurgical slag discrimination method
Study respectively the discriminating research that X-ray diffraction spectroscopic methodology and fourier transform infrared spectroscopy are applied to manganese ore, by research, found out the effective ways that manganese ore and manganese metallurgical slag are differentiated.
The achievement in research of the present invention's research work in early stage acquisition is as follows:
1, found the essential difference of manganese ore and manganese metallurgical slag.
Sum up the production process of current main manganese metallurgical slag: manganese metallurgical slag main source approach has two: the one, produce manganeisen, manganese-silicon and produce the cooling slag of air and Water Quenching Slag; The 2nd, pyrogenic process enrichment, processes that high phosphorus, high ferro difficulty select lean ore and the rich manganese slag that produces.Because of production technology difference, thing phase and composition that manganese metallurgical slag forms are also variant.
2, tentatively set up the X ray diffracting spectrum storehouse of the manganese metallurgical slag that country variant manganese ore, various processes produce.
Propose to set up the conception of country variant manganese ore, manganese metallurgical slag thing phase database, effectively solved manganese ore and manganese metallurgical slag is compared discriminating problem.
3, tentatively set up the Infrared Spectral Database of the manganese metallurgical slag that country variant manganese ore, various processes produce.
The country variant manganese ore of setting up, the conception in manganese metallurgical slag ir data storehouse, effectively proved manganese ore and manganese metallurgical slag is compared discriminating problem.
The taken separately discriminating step of the present invention is as follows:
(1), draw samples quantity is no less than 100g, by the sample splitting of extraction, be crushed to all by 200 eye mesh screens;
(2), take X-ray diffraction spectroscopic methodology to carry out X-ray diffraction spectral analysis to sample
A), by sample in 105 DEG C of oven dry, put into sample box, after compacting, put into X-ray diffraction spectrometer sample chamber, scan and deposit in spectrogram, automatic analysis spectrum peak, stores to be checked;
If b) X-ray diffraction spectral analysis result exists obvious manganese metallurgical slag characteristic spectrum peak, judgement sample attribute is manganese metallurgical slag, otherwise need to carry out next step;
(3), adopt infra-red sepectrometry to carry out Infrared spectroscopy to sample
A), require preparation to detect print according to infrared spectrum sample, put into that spectrum chamber is detected and to record spectrogram to be checked;
If b) the results of FT-IR exists obvious manganese metallurgical slag characteristic, judgement sample attribute is manganese metallurgical slag, otherwise can judge that this sample is manganese ore.
By the research to manganese ore and manganese metallurgical slag Main Differences, think that manganese metallurgical slag is the discarded object producing or contains manganese refining slag in refining manganese and manganese alloy process, the each component concentration of manganese metallurgical slag is all in the corresponding content range of manganese ore, and therefore list cannot be distinguished manganese ore and manganese metallurgical slag from component concentration.Table 1, table 2 have provided the feature of manganese ore and the each component concentration of manganese metallurgical slag.
Table 1 manganese ore chemical component table
Table 2 manganese metallurgical slag typical case chemical component table
w/ %
The manganese mineral phase composition of table 3 main body entrance country origin
The main thing phase composition of table 4 manganese metallurgical slag
Because x ray fluorescence spectrometry only can carry out to sample the judgement of content, and its content can not be made attribute discriminating to manganese ore and manganese metallurgical slag, therefore research adopts X-ray diffraction method and infra-red sepectrometry to find out the thing facial difference of manganese ore and manganese metallurgical slag, thereby distinguishes both.
1.X x ray diffraction analysis x
The X-ray diffraction result MSDS of model Imported Manganese Ore and manganese metallurgical slag.The present invention is to 15 national manganese ores, the manganese metallurgical slag of 3 kinds of different process carries out X diffraction analysis, obtain respectively diffractogram, (see Fig. 1 as an example of Australian manganese ore and the cooling slag of air example, Fig. 2), the X-ray diffraction result MSDS that diffracting spectrum has been set up Imported Manganese Ore and manganese metallurgical slag is by analysis in table 3, table 4.
Manganese metallurgical slag diffraction spectrogram analysis to every country manganese ore, 3 kinds of different process is visible, Imported Manganese Ore is mainly taking pyrolusite, manganese oxide, manganosite, braunite, rhodochrosite and quartz as main, and all manganese ores all have crystalline form, so all have its feature XRD spectra, country variant manganese mineral facies type is as shown in table 3.Manganese metallurgical slag is that the phase character of ferrosilite, clinopyroxene and tephroite is main, or owing to not having crystal habit to cause not having characteristic XRD figure, in table 4, this point is also a distinctive points of manganese metallurgical slag and manganese ore simultaneously, because all manganese ores are all products of spontaneous nucleation, all belong to crystalline solid, and Water Quenching Slag do not have specific crystal formation.Hence one can see that, and manganese metallurgical slag is compared with manganese ore, and its thing phase key distinction is to contain ferrosilite and tephroite, or there is no XRD feature spectrogram.For the Water Quenching Slag that there is no crystalline form, can further be assisted discriminating by diffuse reflectance infrared spectroscopy.
A, manganese ore X diffraction conclusion:
The common feature of Imported Manganese Ore is taking manganese oxide, pyrolusite, manganosite, rhodochrosite, braunite as main, or individualism, or several mixing.Other oxide mainly taking things such as quartz mutually as main.
B, manganese metallurgical slag X diffraction conclusion:
The feature of manganese metallurgical slag is mainly the feature of ferrosilite and tephroite, or does not have characteristic XRD figure.
Produce known following 3 points of principle by manganese metallurgical slag: the first, while producing several alloy of manganese with blast furnace, need in raw material, add silica, after high-temperature fusion, generate the mineral that contain silicate, as ferrosilite.So in the slag that the manganese ore after smelting produces, from the angle analysis of chemical composition, contain a large amount of SiO
2, from the angle analysis of thing phase, all have the mineral containing silicate class.The second, producing in the technique of silicomangan, add raw material rauhkalk and lime, so CaO content is also very high in the manganese metallurgical slag of generation.The 3rd, while producing manganeisen, give off manganese slag, granular for shrend, be at high temperature molten condition, and obtain through shrend chilling, do not form good crystallization, admittedly there is no specific crystalline form, cause not having characteristic XRD spectra.
Therefore just can draw above-mentioned conclusion by X-ray diffraction analysis.
2. ftir analysis
The present invention is to 15 national manganese ores, and the manganese metallurgical slag of 3 kinds of different process carries out Infrared spectroscopy, has obtained respectively infrared spectrogram, taking Australian manganese ore and the cooling slag of air as example (seeing Fig. 3, Fig. 4), and has summed up its infrared signature separately.
The analysis that import is carried out to infrared signature peak from these 15 national manganese ores draws: manganese ore mainly contains the infrared signature of two types: the one, and, at 691cm
-1, 538 cm
-1, 411 cm
-1there is very strong absorption peak at wave number place, is the characteristic peak of manganese oxide; Or at 685cm
-1, 550 cm
-1, 410 cm
-1there is very strong absorption peak at wave number place, is the characteristic peak of pyrolusite, all belongs to the absorption of vibrations of Mn-O, belongs to oxide mineral, at 1000 cm
-1more than do not have characteristic infrared absorption.The 2nd,, at 1420 cm
-1there are wide strong absorption peak, 881 cm in place
-1, 729 cm
-1all there is sharp-pointed absorption at place, is the characteristic peak that contains rhodochrosite, and its ownership is respectively: at 1420 cm
-1near wide strong absorption belongs to C-O stretching vibration, 881 cm
-1what locate is C-O in-plane bending vibration, 729 cm
-1the absorption at place is C-O out-of-plane bending vibration.Because rhodochrosite belongs to carbonate mineral, so there will be the infrared signature absorption peak of obvious C-O vibration, meanwhile, because containing different cationic impacts, characteristic peak has certain displacement.
If this manganese ore belongs to rhodochrosite type, its infrared spectrum is respectively at 1420 cm
-1, 881 cm
-1, 729 cm
-1there is characteristic absorption peak (Fig. 5) clearly at three places, otherwise its characteristic absorption peak is only at 1000 cm
-1below there is strong absorption peak (Fig. 3).These conclusions are consistent with the conclusion of X-ray diffraction.
Manganese metallurgical slag infrared spectrum analysis to 3 kinds of different process is visible, and the manganese metallurgical slag of this three types has identical infrared signature peak, at 960cm
-1near have wide strong absorption peak, and be the strongest absorption band in whole spectrogram.It is attributed to Si-O stretching vibration absorption band.For the Water Quenching Slag that there is no XRD characteristic peak, infrared spectrum also can draw definite conclusion (Fig. 6), has made up the defect of XRD.
A, manganese ore infrared absorption conclusion:
The common feature of Imported Manganese Ore is, only at 600 ~ 400 cm
-1in scope, have two strong absorption bands, bands of a spectrum are wider.Except rhodochrosite is at 1420 cm
-1place has outside characteristic absorption peak, and other type manganese ore is at 1000cm
-1more than there is no strong absorption peak.
B, manganese metallurgical slag infrared absorption conclusion:
The feature of manganese metallurgical slag mainly, at 960cm
-1have the strongest wider absorption peak, meanwhile, the manganese ore that process is smelted is at 1420 cm
-1place does not necessarily have characteristic peak.
By manganese ore and the analyses and comparison of manganese metallurgical slag are studied, both can differentiate by X-ray diffraction and Infrared spectroscopy.Concrete grammar is:
A, sample preparation to be identified: be ground to by 200 mesh sieves, 105 DEG C of oven dry, put into exsiccator and be cooled to room temperature.
B, X-ray diffraction spectroscopic methodology: search the feature that whether has obvious ferrosilite and tephroite in spectrogram, or do not have characteristic XRD figure.Whether can tentatively confirm sample is manganese metallurgical slag.
C, infra-red sepectrometry: whether search in infrared spectrum at 960cm
-1there is the strongest wider absorption peak, and at 1420 cm
-1place does not have characteristic peak, can assist whether confirmation sample is manganese metallurgical slag.
For unknown manganese ore sample identification testing process
The progressively division of the sample of a, extraction, be crushed to all by 200 eye mesh screens
B, by sample in 105 DEG C of oven dry, be placed in exsiccator and be cooled to room temperature
Sample is carried out to X-ray diffraction analysis, as having the feature of obvious ferrosilite and tephroite in sample after testing, or do not have characteristic XRD spectrum peak, can tentatively confirm sample is manganese metallurgical slag, as without this obvious characteristic, needs infrared spectrum to detect.
C, sample is carried out to infrared spectrum detection: whether search in infrared spectrum at 960cm
-1there is the strongest wider absorption peak, and at 1420 cm
-1place does not have characteristic peak, and can confirm sample is manganese metallurgical slag.
Embodiment 1: the qualification of manganese metallurgical slag
First to sample drying and processing, then preparation, by 200 eye mesh screens.
Adopt X-ray diffraction spectral analysis: the sample of selecting is carried out to the spectrum peak of obvious tephroite in X-ray diffraction spectral analysis discovery sample, therefore judge that this sample is manganese metallurgical slag, and be rich manganese slag.
Adopt Infrared spectroscopy: this sample is carried out to Infrared spectroscopy, can find out the characteristic peak that has obvious manganese metallurgical slag, as Fig. 7.Can judge that this sample is manganese metallurgical slag.
According to the above description, can realize the solution of the present invention in conjunction with art technology.
Claims (1)
1. a discrimination method of manganese ore and manganese metallurgical slag being distinguished, is characterized in that: taken separately discriminating step is as follows:
(1), draw samples quantity is no less than 100g, by the sample splitting of extraction, be crushed to all by 200 eye mesh screens;
(2), adopt pressed disc method, adopt X-fluorescence spectrometer to carry out sxemiquantitative scanning to sample, whether preliminary judgement sample belongs to the scope of manganese ore and manganese metallurgical slag, if do not belong to the scope of manganese ore and manganese metallurgical slag, do not belong to the scope that institute's this method is differentiated, if belong to the scope of manganese ore and manganese metallurgical slag, carry out again the analysis of next step;
(3), take X-ray diffraction spectroscopic methodology to carry out X-ray diffraction spectral analysis to sample;
A) sample being placed in to the temperature with 105 DEG C in drying baker dries, then the sample after drying is put into sample box, after compacting, put into X-ray diffraction spectrometer sample chamber, scan and deposit scan-data in spectrogram storehouse through X-ray diffraction spectrometer, by X-ray diffraction spectrometer automatic analysis spectrum peak, obtain a result, data storing is to be checked;
If b) X-ray diffraction spectral analysis result exists obvious manganese metallurgical slag characteristic spectrum peak, judgement sample attribute is manganese metallurgical slag, but not manganese ore, otherwise need to carry out next step;
(4), adopt fourier transform infrared spectroscopy to carry out characteristic infrared absorption spectrum analysis to the sample after step (3) inspection:
A) require preparation to detect sample according to infrared spectrum sample, sample is placed into and in spectrum chamber, detects and to record spectrogram to be checked;
If b) the results of FT-IR exists obvious manganese metallurgical slag characteristic, judgement sample attribute is manganese metallurgical slag, otherwise can judge that this sample is manganese ore.
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| CN106885814A (en) * | 2017-03-07 | 2017-06-23 | 阿拉山口出入境检验检疫局综合技术服务中心 | Copper mine and cupric slightly refining or the discriminating of sintered material attribute |
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| CN107462543A (en) * | 2017-10-09 | 2017-12-12 | 阿拉山口出入境检验检疫局综合技术服务中心 | A kind of detection method that copper mine and copper-contained material are detected based on infra-red sepectrometry |
| CN109211835A (en) * | 2018-10-11 | 2019-01-15 | 南京大学（溧水）生态环境研究院 | A kind of rubbish from cooking rapid identification method based on spectral technique |
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