CN117871570A - Preparation and analysis method of Direct Reduced Iron (DRI) melting piece of hydrogen-based shaft furnace - Google Patents
Preparation and analysis method of Direct Reduced Iron (DRI) melting piece of hydrogen-based shaft furnace Download PDFInfo
- Publication number
- CN117871570A CN117871570A CN202410019550.1A CN202410019550A CN117871570A CN 117871570 A CN117871570 A CN 117871570A CN 202410019550 A CN202410019550 A CN 202410019550A CN 117871570 A CN117871570 A CN 117871570A
- Authority
- CN
- China
- Prior art keywords
- dri
- hydrogen
- reduced iron
- shaft furnace
- direct reduced
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 17
- 239000001257 hydrogen Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000004458 analytical method Methods 0.000 title abstract description 22
- 238000002844 melting Methods 0.000 title description 5
- 230000008018 melting Effects 0.000 title description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000011521 glass Substances 0.000 claims abstract description 9
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005266 casting Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 4
- 238000004846 x-ray emission Methods 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims description 6
- XZXYQEHISUMZAT-UHFFFAOYSA-N 2-[(2-hydroxy-5-methylphenyl)methyl]-4-methylphenol Chemical compound CC1=CC=C(O)C(CC=2C(=CC=C(C)C=2)O)=C1 XZXYQEHISUMZAT-UHFFFAOYSA-N 0.000 claims description 3
- 229940107816 ammonium iodide Drugs 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000010309 melting process Methods 0.000 abstract description 2
- 238000001917 fluorescence detection Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- VJFCXDHFYISGTE-UHFFFAOYSA-N O=[Co](=O)=O Chemical compound O=[Co](=O)=O VJFCXDHFYISGTE-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a preparation and analysis method of a Direct Reduced Iron (DRI) fuse piece of a hydrogen-based shaft furnace, which comprises the following steps: the method comprises the steps of forming an inner sleeve crucible of a platinum yellow crucible by using a lithium tetraborate integrated casting mold, placing the demolded inner sleeve crucible into platinum Huang Ganguo, uniformly mixing 0.2+/-0.01 g of sample, 0.2+/-0.01 g of cobaltosic oxide and 1+/-0.1 g of lithium carbonate, pouring into the inner sleeve crucible, then placing into a muffle furnace for pre-oxidation, cooling, dripping a release agent, preparing a glass sample by high-frequency heating, and analyzing the glass sample by adopting an X-ray fluorescence spectrometry. The method solves the problem of corrosion to the platinum crucible in the direct reduced iron melting process of the DRI of the hydrogen-based shaft furnace, and the prepared sample wafer is smooth and complete and meets the detection requirement.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a preparation and analysis method of a Direct Reduced Iron (DRI) fuse piece of a hydrogen-based shaft furnace.
Background
The DRI direct reduced iron is a green product of a hydrogen-metallurgy hydrogen-based shaft furnace, and is characterized by high grade, low content of S, P harmful elements, high content of metallic iron and less impurities. Because the metal iron content is high, the platinum crucible is easy to corrode to a certain extent during melting, the stripping effect of the fuse piece is poor, the surface is not smooth, the fuse piece is easy to crack, and the detection requirement of an X-ray fluorescence meter is not met.
The fluorescent analysis method is a common quantitative analysis method and has the advantages of simple operation, rapid analysis, high precision and the like. The conventional preparation method of the fusion piece for directly reducing the iron by DRI can not meet the requirement of fluorescence detection, and a sample preparation method which can meet the requirement of fluorescence detection and does not corrode a platinum crucible needs to be developed.
Disclosure of Invention
The invention aims to provide a preparation and analysis method of a Direct Reduced Iron (DRI) fuse piece of a hydrogen-based shaft furnace, which aims to solve the problem of corrosion to a platinum crucible in the direct reduced iron melting process of the DRI of the hydrogen-based shaft furnace, and the prepared sample piece is smooth and complete and meets the detection requirement.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a direct reduced iron melt piece of a hydrogen-based shaft furnace DRI specifically comprises the following steps: the method comprises the steps of forming an inner sleeve crucible of a platinum yellow crucible by using a lithium tetraborate integrated casting mold, placing the demolded inner sleeve crucible into platinum Huang Ganguo, uniformly mixing 0.2+/-0.01 g of sample, 0.2+/-0.01 g of cobaltosic oxide and 1+/-0.1 g of lithium carbonate, pouring the mixture into the inner sleeve crucible, then placing the mixture into a muffle furnace for pre-oxidation, cooling, dripping a release agent, and preparing a glass sample by high-frequency heating.
Further, the lithium tetraborate is used in an amount of 6+ -0.5 g.
Further, the pre-oxidation process of the invention sets the temperature of the muffle furnace to 800+/-50 ℃ and the pre-oxidation time to 20+/-10 min.
Further, the release agent is 50+/-20% of ammonium iodide; the release agent is added in an amount of 10 drops, and the release agent is added in an amount of 1 drop when the titration sucker naturally drops vertically.
The glass sample wafer prepared by the method has smooth, uniform and complete surface.
The invention relates to a method for analyzing Direct Reduced Iron (DRI) melting pieces of a hydrogen-based shaft furnace, which specifically comprises the following steps: the melt was analyzed by X-ray fluorescence spectroscopy.
The beneficial effects of adopting above-mentioned technical scheme to produce lie in:
according to the invention, a mode of forming the platinum crucible by integrally casting lithium tetraborate is adopted, so that the corrosion of a sample to the platinum crucible is avoided, the surface of the prepared glass sample is smooth and uniform, and the fluorescence detection requirement is met.
The method provided by the invention is simple and convenient to operate, rapid in analysis and high in precision, greatly shortens the analysis time, improves the working efficiency, provides powerful data support for subsequent hydrogen metallurgy production, and improves the accuracy of DRI direct reduced iron analysis.
The analysis method has the characteristics of high analysis precision, good reproducibility and reproducibility, ensures normal and orderly production, realizes smooth data transmission, and can meet the requirements of on-line detection and guidance production.
Drawings
FIG. 1 is a graph showing the operation of iron element in the embodiment of the present invention;
FIG. 2 is a graph showing the operation of silicon element in an embodiment of the present invention;
FIG. 3 is a graph showing the working curve of the calcium element in the embodiment of the present invention;
FIG. 4 is a graph showing the operation of magnesium element in the embodiment of the present invention;
FIG. 5 is a graph showing the working curve of titanium element in the embodiment of the present invention;
FIG. 6 is a graph showing the operation of phosphorus in accordance with an embodiment of the present invention;
FIG. 7 is a graph showing the working curve of aluminum element in the embodiment of the present invention;
FIG. 8 is a graph showing the operation of manganese element in the example of the present invention.
Detailed Description
The technical scheme of the invention is further described in detail below by means of examples and with reference to the accompanying drawings.
Examples
A preparation and analysis method of a Direct Reduced Iron (DRI) fuse piece of a hydrogen-based shaft furnace comprises the following steps:
(1) Preparing a fuse piece: forming an inner sleeve crucible of a platinum yellow crucible by using a 6g lithium tetraborate integrated casting mold, placing the demolded inner sleeve crucible into platinum Huang Ganguo, uniformly mixing 0.2g sample, 0.2g cobalt trioxide and 1g lithium carbonate, pouring into the inner sleeve crucible, and then placing into a muffle furnace for pre-oxidation, wherein the pre-oxidation temperature is set to 800 ℃ and the pre-oxidation time is set to 20 min; after cooling, 10 drops (1 drop of the vertical and natural dropping amount of a titration straw) of 50% ammonium iodide are added dropwise as a release agent, and a glass sample is prepared by high-frequency heating; the surface of the glass sample is smooth, uniform and complete.
(2) X-ray fluorescence analysis: registering the standard value of each analysis element of the standard sample, using the prepared standard sample wafer as PHD, registering the intensity, and establishing a working curve, specifically as follows.
A. Selection of standard samples
At present, only one set of commercial direct reduced iron standard samples is available, the content is close, the gradient requirement for establishing a working curve cannot be met, two standard samples with different contents are selected, and meanwhile, standard samples with stable contents of all components are selected, the content requirement is met through proportion, and a certain gradient is formed. The standard samples are shown in Table 1, and the prepared standard samples and the component contents are shown in Table 2.
TABLE 1 Standard sample Meter
Table 2 table of the prepared standard samples
B. Fluorescent analysis conditions
And (3) selecting an element analysis channel and a spectroscopic crystal, and determining pipe flow, pipe pressure, analysis spectral lines, PHA (phase-change) range, analysis time, a goniometer 2 theta angle and the like. The elemental analysis measurement conditions are shown in Table 3.
TABLE 3 elemental analysis measurement conditions
C. Scanning the strength of a standard sample, and manufacturing a correction working curve:
under the determined analysis conditions, the standard sample is scanned, the data processor automatically makes a working curve, and the standard sample is corrected by adopting a fixed a coefficient because the known component content of the standard sample cannot be in the range of 95-105%, and the glass sheet is manufactured by adopting a melting method.
The working curves of the iron element, the silicon element, the calcium element, the magnesium element, the titanium element, the phosphorus element, the aluminum element and the manganese element are sequentially shown in figures 1-8.
(3) Precision testing
A direct reduced DRI sample was selected, 10 replicates were performed according to the above sample melt preparation method and analysis conditions, and the contents of the components were calculated according to the established working curve, and the results are shown in Table 4.
TABLE 4 results of sample parallel assay
(4) Accuracy verification
Samples were prepared according to the fusion method, and a fraction of the DRI samples were analyzed by comparison with the northeast university detection center fluorescence fusion and chemical analysis, and the results are shown in Table 5.
Table 5 data comparison results
As can be seen from tables 4 and 5, the method provided by the invention has higher accuracy and precision.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (5)
1. A preparation method of a direct reduced iron fuse piece of a hydrogen-based shaft furnace DRI is characterized in that an inner crucible of a platinum yellow crucible is formed by integrally casting lithium tetraborate, the demolded inner crucible is placed in platinum Huang Ganguo, 0.2+/-0.01 g of sample, 0.2+/-0.01 g of cobaltosic oxide and 1+/-0.1 g of lithium carbonate are uniformly mixed and poured into the inner crucible, and then the inner crucible is placed into a muffle furnace for pre-oxidation, cooled and then added with a release agent in a dropwise manner, and a glass sample piece is prepared by high-frequency heating.
2. The method for producing a direct reduced iron melt by DRI in a hydrogen-based shaft furnace according to claim 1, wherein the lithium tetraborate is used in an amount of 6±0.5g.
3. The method for preparing the direct reduced iron melt by DRI in the hydrogen-based shaft furnace according to claim 1, wherein the pre-oxidation process is carried out at a muffle temperature of 800+/-50 ℃ for 20+/-10 min.
4. The method for producing a direct reduced iron melt by DRI in a hydrogen-based shaft furnace according to claim 1, wherein: the release agent is 50+/-20% of ammonium iodide.
5. A method for analyzing a molten piece of direct reduced iron by DRI of a hydrogen-based shaft furnace, characterized in that the molten piece prepared in claim 1 is analyzed by an X-ray fluorescence spectrometry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410019550.1A CN117871570A (en) | 2024-01-05 | 2024-01-05 | Preparation and analysis method of Direct Reduced Iron (DRI) melting piece of hydrogen-based shaft furnace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410019550.1A CN117871570A (en) | 2024-01-05 | 2024-01-05 | Preparation and analysis method of Direct Reduced Iron (DRI) melting piece of hydrogen-based shaft furnace |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117871570A true CN117871570A (en) | 2024-04-12 |
Family
ID=90586081
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410019550.1A Pending CN117871570A (en) | 2024-01-05 | 2024-01-05 | Preparation and analysis method of Direct Reduced Iron (DRI) melting piece of hydrogen-based shaft furnace |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117871570A (en) |
-
2024
- 2024-01-05 CN CN202410019550.1A patent/CN117871570A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101526488A (en) | Method for analyzing components of iron ore by using X-ray fluorescence spectrum | |
| CN102368052B (en) | Preparation method of copper alloy spectral standard sample | |
| CN102156142A (en) | Method for analyzing ferrosilicon alloy components for X-ray fluorescence spectrum analysis | |
| CN101149333A (en) | Spectrum standard sample for detecting coin-manufacturing non-corrosive steel and its manufacture method | |
| CN103149074A (en) | Molten sample preparation method of molybdenum, manganese, vanadium or chromium iron alloy sample for X-ray fluorescence spectroscopy | |
| CN103604823A (en) | Method for measuring contents of potassium, sodium, lead and zinc in iron ore | |
| CN106442073A (en) | Fusion sample preparation method for X-ray fluorescence analysis of element contents of silicon and phosphorus in silicon-manganese ball alloy | |
| CN110261420A (en) | The method of x-ray fluorescence spectrometry serpentine chemical component | |
| CN111855722B (en) | MgO and SiO in light-burned magnesium and magnesium stone 2 X-ray fluorescence spectrum analysis method of content | |
| CN102331364A (en) | Melted sampling method for aluminum magnesium calcium iron alloy for X-ray fluorescence spectrum analysis | |
| CN108254234A (en) | A kind of preparation method of stainless steel smelting process control standard specimen | |
| CN114486968A (en) | Method for measuring contents of titanium, silicon, manganese, phosphorus, aluminum and copper in ferrotitanium by dissolution-melting method sample preparation-X-ray fluorescence spectrometry | |
| CN106338534B (en) | The method of Calcium Fluoride Content in fluorite is quickly measured using Xray fluorescence spectrometer | |
| CN112051290B (en) | Ferromolybdenum sample, preparation method thereof and method for measuring component content in ferromolybdenum alloy | |
| CN113295676A (en) | Method for measuring calcium, aluminum and barium in deoxidizer | |
| CN117871570A (en) | Preparation and analysis method of Direct Reduced Iron (DRI) melting piece of hydrogen-based shaft furnace | |
| CN106290438B (en) | A kind of method that X-ray fluorescence spectra fusion method measures Calcium Fluoride Content in fluorite | |
| CN112461878B (en) | Method for measuring content of ferronickel in carbonyl ferronickel alloy powder | |
| CN111272737A (en) | Method for determining percentage content of multiple elements in high-silicon aluminum alloy through microwave digestion-ICP-OES and application of method | |
| CN110646452A (en) | Method for measuring major elements in ferrochrome alloy by X fluorescence fuse link method | |
| CN104677701A (en) | Preparation method of standardized sample for X-ray fluorescence analysis | |
| CN105784746A (en) | Method for detecting ferrosilicon element by combing graphite crucible sample melting with X-ray fluorescence | |
| CN112683621A (en) | Method for detecting content of silicon element in manganese-silicon alloy | |
| CN111239172A (en) | Method for determining phosphorus content in coal | |
| CN108956259B (en) | Method for detecting free carbon in continuous casting mold flux |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |