CN-122016897-A - Method for detecting TiC in stokehole carbide slag

Abstract

The invention belongs to the chemical field, and relates to a method for detecting TiC in stokehole carbide slag, which comprises the following steps of S10, establishing a standard working curve, namely (a) uniformly mixing an internal standard Y 2 O 3 with a series of carbonized slag standard samples with known TiC content according to a fixed mass ratio to obtain a series of mixed standard samples, (b) respectively scanning the mixed standard samples under the same test condition by adopting an X-ray diffractometer to obtain a corresponding X-ray diffraction pattern, (c) identifying and measuring the characteristic diffraction peak intensity I TiC of TiC and the characteristic diffraction peak intensity I Y2O3 of the internal standard Y 2 O 3 , (d) calculating the corresponding intensity ratio R i =I TiC /I Y2O3 of each standard sample, and (e) linearly fitting to obtain the standard working curve, and S20, measuring the sample to be detected. The detection method is simple, convenient and high in accuracy.

Inventors

• WANG DONGSHENG
• LV XUEMING
• LI LIANG
• LU RUIFANG

Assignees

• 攀钢集团攀枝花钢铁研究院有限公司

Dates

Publication Date

20260512

Application Date

20260225

Claims (10)

1. 1. The method for detecting TiC in the stokehold carbide slag is characterized by comprising the following steps of: s10, establishing a standard working curve: (a) Uniformly mixing an internal standard Y 2 O 3 with a series of carbonized residue standard samples with known TiC content according to a fixed mass ratio to prepare a series of mixed standard samples; (b) Respectively scanning the mixed standard sample under the same test condition by adopting an X-ray diffractometer to obtain a corresponding X-ray diffraction pattern; (c) Identifying and measuring the characteristic diffraction peak intensity I TiC of TiC and the characteristic diffraction peak intensity I Y2O3 of an internal standard Y 2 O 3 respectively from each X-ray diffraction pattern; (d) Calculating the intensity ratio R i =I TiC /I Y2O3 corresponding to each standard sample; (e) Taking the known TiC content as an abscissa and the corresponding intensity ratio R i as an ordinate, performing linear fitting to obtain a standard working curve; S20, measuring a sample to be measured: (f) Uniformly mixing the internal standard Y 2 O 3 with the carbide slag sample to be detected according to the fixed mass ratio same as that in the step (a) to prepare a mixed sample to be detected; (g) Under the same test condition as in the step (b), carrying out X-ray diffraction scanning on the mixed sample to be tested to obtain an X-ray diffraction pattern of the mixed sample; (h) Measuring the characteristic diffraction peak intensities I TiC and I Y2O3 of the characteristic diffraction peaks of Y 2 O 3 of TiC from the X-ray diffraction spectrum of the mixed sample to be detected, and calculating the intensity ratio R x ; (i) Substituting the intensity ratio R x into the standard working curve, and calculating the TiC content in the carbide slag sample to be detected.
2. 2. The method according to claim 1, wherein in the steps (a) and (f), the fixed mass ratio of the carbonized residue sample to the internal standard Y 2 O 3 is (2-3): 1.
3. 3. The method according to claim 1, wherein in the step (a), the content of TiC in the series of carbonized residue standard samples covers a mass fraction range of 2% to 15%.
4. 4. A detection method according to claim 3, wherein the series of carbide slag standard samples comprises at least five different content points of TiC of 2%, 4%, 6%, 8%, 10%, 12%, 14% and 15% by mass.
5. 5. The method according to claim 1, wherein in steps (c) and (h), the characteristic diffraction peak of TiC is selected from diffraction peaks having a2Θ of 41.9 ° ± 0.2 °.
6. 6. The method of claim 1, wherein in steps (c) and (h), the characteristic diffraction peak of the internal standard Y 2 O 3 is selected from diffraction peaks having a2Θ of 48.5 ° ± 0.2 °.
7. 7. The method according to claim 1, wherein in the steps (b) and (g), the same test conditions include a scanning range 2. Theta. Of an X-ray diffractometer of 10 DEG to 90 deg.
8. 8. The method of claim 1, wherein in steps (a) and (f), the uniform mixing comprises performing sufficient grinding in a mortar.
9. 9. The method of claim 1, wherein in steps (a) and (f), the prepared mixed powder sample is subjected to a leveling process after being loaded into the sample holder to ensure uniformity of the flatness of the test surface.
10. 10. The method of claim 1, wherein the internal standard Y 2 O 3 is an analytically pure reagent.

Description

Method for detecting TiC in stokehole carbide slag Technical Field The invention belongs to the field of chemistry, and relates to a method for detecting TiC in stokehole carbide slag. Background Titanium resources in Sichuan Panxi area are abundant, most of titanium enters blast furnace slag through the traditional blast furnace ironmaking-converter steelmaking process, and the content of TiO 2 in the blast furnace slag is 20% -26%. Aiming at blast furnace slag, many research institutions in China have conducted researches on various titanium extraction technical routes, such as preparation of silicon-titanium composite alloy, production of slag glass ceramics and the like, but the treatment capacity is limited, and the comprehensive utilization problem of titanium-containing blast furnace slag cannot be fundamentally solved. At present, the technological route for preparing TiCl 4 from high-titanium blast furnace slag through high-temperature carbonization-low-temperature chlorination is the technological route with the most industrialization prospect. The high-temperature carbonization process adopts an electric furnace to smelt high-titanium blast furnace slag, namely, tiO 2 in the slag is reduced by carbon powder, and along with the smelting, tiO 2 in the slag is gradually converted into TiC, and when the smelting is close to the end point, the TiC content in the slag is about 15%, so that the slag is named as carbonized slag. Currently, chemical analysis methods are adopted for measuring TiC content in the carbide slag, including spectrophotometry, X-ray fluorescence spectrometry and other treatment methods. For example, chinese patent CN112266020B provides an accurate method for measuring titanium carbide in carbide slag, aiming at the problems of easy hydrolysis of titanium, inaccurate measurement result and poor reproducibility in the existing method for measuring titanium carbide in carbide slag. And adding EDTA solution when dissolving the carbide slag sample, and keeping the volume of the solution at 25-40 mL when dissolving. The method can effectively prevent the titanium ions generated by decomposing titanium carbide with nitric acid from hydrolyzing again, so that the operability of the analysis method is greatly improved, and the analysis accuracy is improved. The chemical method has the following defects that the sample preparation, dissolution, separation and other working procedures are needed, the measurement usually needs more than 2 hours, the analysis result cannot be fed back in time to guide the high-temperature carbonization smelting control, the chemical analysis sample is small, the measurement dosage is only 0.1-0.2 g, the error is relatively large when the segregated carbonized slag is analyzed, a large amount of acid solution, hydrofluoric acid, nitric acid and the like are needed in the analysis process, and the environment is easy to be polluted. Therefore, a method for rapidly detecting the TiC content in the carbide slag is required to be sought and used for guiding the judgment of the smelting end point in front of the furnace. Disclosure of Invention In view of the above, the invention provides a method for detecting TiC in stokehole carbide slag, which aims to quantitatively analyze the carbide slag by XRD by adopting an internal standard method and solves the technical problems that the existing method for measuring the TiC content in the carbide slag consumes long time and cannot be used for guiding stokehole smelting endpoint judgment. In order to solve at least one of the technical problems, the invention adopts the following technical scheme: The invention provides a method for detecting TiC in stokehole carbide slag, which comprises the following steps of S10, establishing a standard working curve, (a) uniformly mixing an internal standard Y 2O3 with a series of carbide slag standard samples with known TiC content according to a fixed mass ratio to obtain a series of mixed standard samples, (b) adopting an X-ray diffractometer to respectively scan the mixed standard samples under the same test condition to obtain corresponding X-ray diffraction patterns, (c) respectively identifying and measuring the characteristic diffraction peak intensity I TiC of TiC and the characteristic diffraction peak intensity I Y2O3 of an internal standard Y 2O3 from the X-ray diffraction patterns, (d) calculating the corresponding intensity ratio R i=ITiC/IY2O3 of each standard sample, taking the known TiC content as an abscissa and taking the corresponding intensity ratio R i as an ordinate to obtain a standard working curve, (S20, measuring the internal standard Y 2O3 and the carbon slag sample to be measured according to the same fixed mass ratio as the standard sample in the step (a)), obtaining the mixed characteristic diffraction peak intensity I TiC of TiC and the characteristic diffraction peak I 2O3 of the internal standard sample to be measured from the X-ray diffraction patt