CN104198514B - Manganese ore and manganese metallurgical slag attribute discrimination method - Google Patents
Manganese ore and manganese metallurgical slag attribute discrimination method Download PDFInfo
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Abstract
The present invention relates to a kind of manganese ore and manganese metallurgical slag attribute discrimination method, the method is respectively adopted X-ray diffraction spectra method, infrared spectrometry, manganese ore and manganese metallurgical slag are carried out attribute discriminating, by the X-ray diffraction spectra lookup to feature spectral peaks such as the pyrolusite in manganese ore, manganese oxide, manganosite, manganese spars, and with the analysis contrast of the characteristic peak such as the ferrosilite of manganese metallurgical slag, manganese ore attribute is differentiated, simultaneously, can be proved by infrared spectrum feature, manganese ore is at 600 ~ 400cm‑1In the range of have two strong absorption bands, and individually or simultaneously at 1420cm‑1There is characteristic absorption peak at place, and manganese metallurgical slag is at 960cm‑1Neighbouring wide strong absworption peak, can carry out manganese ore attribute confirming to differentiate simultaneously, and this authentication method is inspection and quarantine, customs's offer technical support, provides the probation report of science for trade people, it is ensured that border safety, it is to avoid environmental pollution and trade fraud.
Description
Technical field
The present invention relates to the discrimination method of manganese ore, particularly to 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 pair
Manganese ore differentiates with manganese metallurgical slag attribute.
Background technology
Manganese ore refers to the manganese-bearing mineral that natural conditions are formed, and is mainly used in refining the purposes of manganese.In modern industry, manganese and
Its compound is applied to the every field of national economy, and wherein steel and iron industry is most important field, accounts for 90%～95% by manganese amount,
Mainly as the deoxidizer in ironmaking and steelmaking process and desulfurizing agent, and it is used for manufacturing alloy.China is the Eleventh Five-Year Plan period
Manganese is listed national strategy resource in, it is seen that manganese ore has highly important strategic position.Therefore, increasing enterprise, public affairs
Department has carried out the foreign trade of manganese ore.
Under market, cause unordered competition, pursued maximum profit, cause domestic and international illegal retailer with secondary
Substituting the bad for the good, pass a fake product off as a genuine one, the phenomenon of the melting waste slag of doping China nonimportation constantly occurs, has had a strong impact on the trade ring of China
Border, compromises the interests of importer, and the ecological environment to China simultaneously causes heavy damage.Manganese mud is with silicon, the oxidation of calcium
Thing is main, and Fe content is relatively low, smelt be worth the lowest, and containing a large amount of poisonous and harmful heavy metallics, such as lead, zinc, arsenic, copper, above-mentioned
Harmful heavy metal meeting polluted surface water, subsoil water and soil, do great damage to ecological environment.
And owing to manganese metallurgical slag has similar elementary composition and content to some manganese ores, list is from the height of constituent content sometimes
Cannot accurately be distinguished.China does not still have effective manganese ore and manganese metallurgical slag discrimination method at present so that the departments such as customs look into
Place causes considerable trouble, so urgently setting up effective discrimination method of manganese ore and metallurgical slag thereof, preferably safeguards national economic interest, guarantor
Protect country's ecological environment.
Summary of the invention
The purpose of the present invention, exactly for overcoming the deficiencies in the prior art, differentiates a difficult problem for manganese ore and manganese metallurgical slag, it is provided that
A kind of effectively discrimination method, goes through a few year, by the relevant attribute of manganese ore, manganese metallurgical slag being differentiated, mass data is received
Collection, and the data of collection is sorted out, by contrast after analysis and research, the most successfully find out a kind of manganese ore and manganese metallurgical slag
Attribute discrimination method；Meanwhile, this method is taked can to serve inspection and quarantine, customs, R&D institution, universities and colleges, inspection center
And between corresponding manufacturer, the classification of the waste and old material mineral to import class such as department differentiates, is hindered by technological means
Only industrial refuse immigration, has ensured China's Environmental security.
The present invention is realized by such technical scheme: a kind of discriminating side made a distinction manganese ore with manganese metallurgical slag
Method, it is characterised in that: taken separately discriminating step is as follows:
(1), extraction sample size no less than 100g, by the sample splitting of extraction, be crushed to all by 200 eye mesh screens；
(2), using pressed disc method, use X fluorescence spectrometer that sample is carried out sxemiquantitative scanning, whether preliminary judgement sample
Belonging to manganese ore and the scope of manganese metallurgical slag, if being not belonging to manganese ore and the scope of manganese metallurgical slag, being then not belonging to the discriminating of this method
Scope, if belonging to manganese ore and the scope of manganese metallurgical slag, carries out the analysis of next step the most again；
(3), take X-ray diffraction spectra method that sample is carried out X-ray diffraction spectra analysis；
Drying with the temperature of 105 DEG C in a) sample is placed in drying baker, the sample after then drying is put in sample box,
Put in X-ray diffraction spectrometer sample room after compacting, scan through X-ray diffraction spectrometer and scan data be stored in spectrogram storehouse, by X
X ray diffraction spectrometer automatically analyzes spectral peak, obtains a result, and data is stored to be checked；
If b) there is obvious manganese metallurgical slag feature spectral peak, then judgement sample attribute in X-ray diffraction spectra analysis result
For manganese metallurgical slag, rather than manganese ore, otherwise need to carry out next step；
(4), use fourier transform infrared spectroscopy that the sample after step (3) is checked is carried out characteristic infrared absorption spectrum
Map analysis:
A) requiring preparation detection sample according to infrared spectrum sample, sample is placed in spectrum room to detect and record spectrogram and treats
Look into；
If b) the results of FT-IR exists obvious manganese metallurgical slag characteristic, then judgement sample attribute is manganese metallurgical slag, no
Then may determine that this sample is manganese ore.
The invention have the advantages that:
Clearly propose manganese ore and manganese metallurgical slag comparison authentication technique.With technical measures as means, with Supervision Measures as mesh
Mark, this authentication method has reached to block imported goods from source and has renamed the purpose made a breakthrough, and provides technology to prop up for inspection and quarantine, customs
Hold, the probation report of science is provided for trade people, it is ensured that border safety, it is to avoid environmental pollution.
Accompanying drawing explanation
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 (air cooling slag) infrared spectrogram；
Fig. 5 is the infrared signature spectrogram of manganese spar；
Fig. 6 is the infrared signature spectrogram of manganese metallurgical slag (Water Quenching Slag)；
The infrared signature spectrogram of Fig. 7 manganese metallurgical slag (Mn-rich slag).
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described.
Early stage research work of the present invention mainly includes the following aspects:
1, research manganese ore and manganese metallurgical slag diversity
Comprehensive collection, arrange domestic and international manganese ore, the classification of manganese metallurgical slag, specification, understand manganese ore production and processing technology, clearly what
Plant which kind of manganese metallurgical slag is production technology will produce, thus find out both essence difference, clearly differentiate directivity target.
2, research manganese ore and manganese metallurgical slag discrimination method
Have studied X-ray diffraction spectra method respectively and fourier transform infrared spectroscopy be applied to the Study on Identification of manganese ore,
By research, have found the effective ways that manganese ore differentiates with manganese metallurgical slag.
The achievement in research that early stage research work of the present invention obtains is as follows:
1, have found the essential difference of manganese ore and manganese metallurgical slag.
Sum up the generation process of manganese metallurgical slag currently mainly: manganese metallurgical slag main source approach has and two: one is
Produce manganeisen, manganese-silicon and produce air cooling slag and Water Quenching Slag；Two is pyrogenic process enrichment, processes high phosphorus, the choosing of high ferro difficulty
Lean ore and the Mn-rich slag that produces.Because production technology is different, thing phase and composition that manganese metallurgical slag is formed are the most variant.
2, the X ray diffracting spectrum of the manganese metallurgical slag of country variant manganese ore, various processes generation is tentatively established
Storehouse.
Propose and set up country variant manganese ore, the conception in manganese metallurgical slag thing phase data storehouse, effectively solve manganese ore and manganese
Metallurgical slag comparison differentiates problem.
3, the Infrared Spectral Database of the manganese metallurgical slag of country variant manganese ore, various processes generation is tentatively established.
The country variant manganese ore of foundation, the conception in manganese metallurgical slag ir data storehouse, effectively proved manganese ore and manganese
Metallurgical slag comparison differentiates problem.
The present invention taken separately discriminating step is as follows:
(1), extraction sample size no less than 100g, by the sample splitting of extraction, be crushed to all by 200 eye mesh screens；
(2), take X-ray diffraction spectra method that sample is carried out X-ray diffraction spectra analysis
A), by sample in 105 DEG C of drying, put in sample box, put into after compacting in X-ray diffraction spectrometer sample room, sweep
Retouch and be stored in spectrogram, automatically analyzing spectral peak, storing to be checked；
If b) there is obvious manganese metallurgical slag feature spectral peak, then judgement sample attribute in X-ray diffraction spectra analysis result
For manganese metallurgical slag, otherwise need to carry out next step；
(3), use infrared spectrometry that sample is carried out infrared spectrum analysis
A), according to infrared spectrum sample require preparation detection print, put into and spectrum room is detected and to record spectrogram to be checked；
If b) the results of FT-IR exists obvious manganese metallurgical slag characteristic, then judgement sample attribute is manganese metallurgical slag, no
Then may determine that this sample is manganese ore.
By to manganese ore and the research of manganese metallurgical slag Main Differences, it is believed that manganese metallurgical slag is during refining manganese and manganese alloy
The garbage produced or the refining slag in manganese, each constituent content of manganese metallurgical slag is all in the corresponding content range of manganese ore, therefore single from group
Divide and cannot be distinguished by manganese ore and manganese metallurgical slag on content.Table 1, table 2 give the feature of manganese ore and each constituent content of manganese metallurgical slag.
Table 1 manganese ore chemical component table
Table 2 manganese metallurgical slag Exemplary chemical component list w/%
The manganese mineral phase composition of table 3 main body entrance country origin
Table 4 manganese metallurgical slag dominant phase composition
Owing to X-ray fluorescence spectroscopy is only capable of carrying out sample the judgement of content, and its content can not be to manganese ore and manganese
Metallurgical slag is made attribute and is differentiated, therefore research uses X-ray diffraction method and infrared spectrometry to find out manganese ore and the thing of manganese metallurgical slag
Facial difference, thus distinguish both.
1.X x ray diffraction analysis x
Initially set up the X-ray diffraction result data sheet of Imported Manganese Ore and manganese metallurgical slag.The present invention is to 15 national manganese
Ore deposit, the manganese metallurgical slag of 3 kinds of different process carries out X diffraction analysis, obtains diffraction pattern respectively, cold with Australia's manganese ore and air
But (see Fig. 1, Fig. 2) as a example by slag, the X-ray diffraction result data of Imported Manganese Ore and manganese metallurgical slag is established through analyzing diffracting spectrum
Table is shown in Table 3, table 4.
Analyzing visible to the manganese metallurgical slag diffraction spectrogram of every country manganese ore, 3 kinds of different process, Imported Manganese Ore is mainly with soft
Manganese ore, manganese oxide, manganosite, braunite, manganese spar and quartz are main, and all manganese ores all have crystal form, so it is special to be respectively provided with it
Levying XRD spectra, country variant manganese mineral facies type is as shown in table 3.Manganese metallurgical slag is ferrosilite, clinopyroxene and tephroite
Phase character is main, or owing to not having crystal habit to cause the XRD figure not having feature, is shown in Table 4, and this point is also simultaneously
One distinctive points of manganese metallurgical slag and manganese ore, because all manganese ores are all the products of spontaneous nucleation, all belongs to crystalline solid, and shrend
Slag does not has specific crystal formation.It follows that manganese metallurgical slag is compared with manganese ore, its thing differs primarily in that mutually containing ferrosilite and manganese olive
Olive stone, or there is no XRD feature spectrogram.For there is no the Water Quenching Slag of crystal form, can further by infrared spectrum feature in addition
Auxiliary differentiates.
A, manganese ore X diffraction conclusion:
The common feature of Imported Manganese Ore is based on manganese oxide, pyrolusite, manganosite, manganese spar, braunite, or individually deposits
, or several mixing.Other oxide is mainly based on things such as quartz mutually.
B, manganese metallurgical slag X diffraction conclusion:
The feature of manganese metallurgical slag is mainly the feature of ferrosilite and tephroite, or does not has the XRD figure of feature.
Produced principle by manganese metallurgical slag and understand following three points: first, during with several alloy of blast fumance manganese, need former
Material adds Silicon stone, after high-temperature fusion, generates the mineral containing silicate, such as ferrosilite.So the manganese ore after smelting
In the slag produced, the chemically angle analysis of composition, containing a large amount of SiO2, from the angle analysis of thing phase, all have containing silicate class
Mineral.Second, in the technique producing silicomangan, add raw material dolomite and Calx, so, the manganese metallurgical slag of generation
Middle CaO content is the highest.3rd, when producing manganeisen, give off manganese slag, granular for shrend, the most at high temperature in molten
State, and obtain through shrend chilling, it is formed without good crystallization, admittedly there is no specific crystal form, causes the XRD spectra not having feature.
Therefore above-mentioned conclusion can just be drawn by X-ray diffraction analysis.
2. ftir analysis
The present invention carries out infrared spectrum analysis to 15 national manganese ores, the manganese metallurgical slag of 3 kinds of different process, obtains respectively
Infrared spectrogram, as a example by Australia's manganese ore and air cooling slag (see Fig. 3, Fig. 4), and summarizes its respective infrared spy
Levy.
The analysis that from these 15 national manganese ores, import is carried out infrared signature peak draws: manganese ore mainly has two kinds of
Infrared signature: one is, at 691cm-1、538 cm-1、411 cm-1There is the strongest absworption peak at wave number, be the characteristic peak of manganese oxide；
Or at 685cm-1、550 cm-1、410 cm-1There is the strongest absworption peak at wave number, be the characteristic peak of pyrolusite, all belong to
The absorption of vibrations of Mn-O, belongs to oxide mineral, at 1000 cm-1More than there is no the INFRARED ABSORPTION of feature.Two are, 1420
cm-1There are wide strong absworption peak, 881 cm in place-1、729 cm-1All there is sharp-pointed absorption at place, is the characteristic peak containing manganese spar, its ownership
It is respectively as follows: at 1420 cm-1Neighbouring wide strong absorption belongs to C-O stretching vibration, 881 cm-1Place for C-O in-plane bending vibration,
729 cm-1The absorption at place is C-O out-of-plane bending vibration.Because manganese spar belongs to carbonate mineral, so there will be obvious C-O
The infrared signature absworption peak of vibration, meanwhile, because of the impact containing different cationes, characteristic peak has certain displacement.
If this manganese ore belongs to manganese spar type, then its infrared spectrum is respectively at 1420 cm-1、881 cm-1、729 cm-1Three
There is characteristic absorption peak (Fig. 5) clearly at place, and otherwise, its characteristic absorption peak is only at 1000 cm-1Hereinafter there is strong absworption peak (Fig. 3).
These conclusions are consistent with the conclusion of X-ray diffraction.
Analyzing visible to the manganese metallurgical slag infrared spectrum of 3 kinds of different process, the manganese metallurgical slag of these three type has identical
Infrared signature peak, i.e. at 960cm-1Near have wide strong absworption peak, and be absorption band the strongest in whole spectrogram.It is attributed to
Si-O stretching vibration absorption band.For not having the Water Quenching Slag of XRD characteristic peak, infrared spectrum also can draw the conclusion (Fig. 6) determined,
Compensate for the defect of XRD.
A, manganese ore INFRARED ABSORPTION conclusion:
The common feature of Imported Manganese Ore is, only at 600 ~ 400 cm-1In the range of have two strong absorption bands, bands of a spectrum are wider.Remove
Manganese spar is at 1420 cm-1Place has outside characteristic absorption peak, and other type manganese ore is at 1000cm-1More than there is no strong absworption peak.
B, manganese metallurgical slag INFRARED ABSORPTION conclusion:
The feature of manganese metallurgical slag is mainly, at 960cm-1There is the strongest wider absworption peak, exist through the manganese ore smelted meanwhile
1420 cm-1Place does not necessarily have characteristic peak.
By research of analysing and comparing manganese ore and manganese metallurgical slag, both can pass through X-ray diffraction and infrared spectrum analysis
Differentiate.Method particularly includes:
A, sample treatment to be identified: be ground to, by 200 mesh sieves, 105 DEG C of drying, put into and in exsiccator, be cooled to room temperature.
B, X-ray diffraction spectra method: search the feature whether having obvious ferrosilite and tephroite in spectrogram, or do not have
There is the XRD figure of feature.Can tentatively confirm whether sample is manganese metallurgical slag.
C, infrared spectrometry: whether search in infrared spectrum at 960cm-1There is the strongest wider absworption peak, and 1420
cm-1Place does not has characteristic peak, can assist whether confirmation sample is manganese metallurgical slag.
For unknown manganese ore sample identification testing process
A, the sample progressively division of extraction, it is crushed to all by 200 eye mesh screens
B, by sample in 105 DEG C of drying, be placed in exsiccator and be cooled to room temperature
Sample is carried out X-ray diffraction analysis, as sample after testing has the feature of obvious ferrosilite and tephroite,
Or not having the XRD spectral peak of feature, can tentatively confirm sample is manganese metallurgical slag, as without this obvious characteristic, needs infrared spectrum to carry out
Detection.
C, sample is carried out infrared spectrum detection: whether search in infrared spectrum at 960cm-1There is wider absorbing the most by force
Peak, and at 1420 cm-1Place does not has 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 prepare, by 200 eye mesh screens.
Employing X-ray diffraction spectra is analyzed: the sample selected carries out X-ray diffraction spectra analysis and finds in sample obvious
The spectral peak of tephroite, therefore judge that this sample is manganese metallurgical slag, and be Mn-rich slag.
Use infrared spectrum analysis: this sample is carried out infrared spectrum analysis, it can be seen that have obvious manganese metallurgical slag
Characteristic peak, such as Fig. 7.May determine that this sample is manganese metallurgical slag.
According to the above description, the solution of the present invention can be realized in conjunction with art technology.
Claims (1)
1. the discrimination method that manganese ore is made a distinction with manganese metallurgical slag, it is characterised in that: taken separately discriminating step is such as
Under:
(1), extraction sample size no less than 100g, by the sample splitting of extraction, be crushed to all by 200 eye mesh screens；
(2), using pressed disc method, use X fluorescence spectrometer that sample carries out sxemiquantitative scanning, whether preliminary judgement sample belongs to
Manganese ore and the scope of manganese metallurgical slag, if being not belonging to manganese ore and the scope of manganese metallurgical slag, be then not belonging to the scope that this method differentiates,
If belonging to manganese ore and the scope of manganese metallurgical slag, carry out the analysis of next step the most again；
(3), take X-ray diffraction spectra method that sample is carried out X-ray diffraction spectra analysis；
Drying with the temperature of 105 DEG C in a) sample is placed in drying baker, the sample after then drying is put in sample box, compacting
After put in X-ray diffraction spectrometer sample room, through X-ray diffraction spectrometer scanning and scan data is stored in spectrogram storehouse, by X-ray
Diffraction screen automatically analyzes spectral peak, obtains a result, and data is stored to be checked；
If b) X-ray diffraction spectra analysis result exists manganese metallurgical slag feature spectral peak, then judgement sample attribute is manganese metallurgical slag,
Rather than manganese ore, otherwise needing to carry out next step, the feature of manganese metallurgical slag is mainly the feature of ferrosilite and tephroite, or
There is no the XRD figure of feature；
(4), use fourier transform infrared spectroscopy that the sample after step (3) is checked is carried out characteristic infrared absorption spectrogram to divide
Analysis:
A) requiring preparation detection sample according to infrared spectrum sample, sample is placed in spectrum room and detects and to record spectrogram to be checked；
If b) the results of FT-IR exists manganese metallurgical slag characteristic, then judgement sample attribute is manganese metallurgical slag, otherwise may determine that
This sample is manganese ore, and the feature of manganese metallurgical slag is mainly, at 960cm-1There is the strongest wider absworption peak, meanwhile, through smelt
Manganese ore is at 1420 cm-1Place does not necessarily have characteristic peak.
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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 |
| CN107389397A (en) * | 2017-06-30 | 2017-11-24 | 包头钢铁（集团）有限责任公司 | A kind of preparation method of manganese metal chemical analysis sample |
| 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 |
| CN109211835B (en) * | 2018-10-11 | 2020-12-01 | 南京大学（溧水）生态环境研究院 | Kitchen waste rapid identification method based on spectrum technology |
| CN112903735A (en) * | 2020-12-21 | 2021-06-04 | 南昌海关技术中心 | Method for rapidly identifying solid waste property of copper concentrate and smelting slag thereof |
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