CN114137017B - Evaluation method for influence of slag volatilization containing volatile components on melting point - Google Patents
Evaluation method for influence of slag volatilization containing volatile components on melting point Download PDFInfo
- Publication number
- CN114137017B CN114137017B CN202111417614.6A CN202111417614A CN114137017B CN 114137017 B CN114137017 B CN 114137017B CN 202111417614 A CN202111417614 A CN 202111417614A CN 114137017 B CN114137017 B CN 114137017B
- Authority
- CN
- China
- Prior art keywords
- slag
- melting point
- volatile components
- heating rate
- volatilization
- 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.)
- Active
Links
- 239000002893 slag Substances 0.000 title claims abstract description 312
- 238000002844 melting Methods 0.000 title claims abstract description 222
- 230000008018 melting Effects 0.000 title claims abstract description 222
- 238000011156 evaluation Methods 0.000 title description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 86
- 238000000034 method Methods 0.000 claims abstract description 41
- 238000005259 measurement Methods 0.000 claims description 34
- 230000008859 change Effects 0.000 claims description 19
- 230000000694 effects Effects 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 6
- 238000004455 differential thermal analysis Methods 0.000 claims description 3
- 238000000691 measurement method Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 abstract description 17
- 238000013213 extrapolation Methods 0.000 abstract description 9
- 229910052731 fluorine Inorganic materials 0.000 description 26
- 239000011737 fluorine Substances 0.000 description 26
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 22
- 238000006243 chemical reaction Methods 0.000 description 20
- 239000000203 mixture Substances 0.000 description 20
- 239000000126 substance Substances 0.000 description 15
- 238000012937 correction Methods 0.000 description 12
- 230000009467 reduction Effects 0.000 description 11
- 230000008569 process Effects 0.000 description 10
- 239000003153 chemical reaction reagent Substances 0.000 description 6
- 230000008878 coupling Effects 0.000 description 6
- 238000010168 coupling process Methods 0.000 description 6
- 238000005859 coupling reaction Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000009853 pyrometallurgy Methods 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000009628 steelmaking Methods 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000009529 body temperature measurement Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910004261 CaF 2 Inorganic materials 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000914 Mn alloy Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- PIRCGUMCHJTHIE-UHFFFAOYSA-N [O].[Na].[K] Chemical compound [O].[Na].[K] PIRCGUMCHJTHIE-UHFFFAOYSA-N 0.000 description 1
- CTNCAPKYOBYQCX-UHFFFAOYSA-N [P].[As] Chemical compound [P].[As] CTNCAPKYOBYQCX-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- -1 alkali metal alkaline earth metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/10—Supplying or treating molten metal
- B22D11/11—Treating the molten metal
- B22D11/111—Treating the molten metal by using protecting powders
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/18—Electroslag remelting
Abstract
The invention belongs to the field of metallurgical engineering, and particularly discloses a method for evaluating the influence of slag volatilization containing volatile components on a melting point, which comprises the following steps: measuring melting points of slag containing volatile components and slag without volatile components under different heating rates to obtain two corresponding relation curves of the melting points and the heating rates; extrapolation is carried out according to the two curves to obtain two melting point values when the temperature rising rate is 0; the corresponding relation curve of the melting point of the slag without volatile components and the heating rate is downwards moved to a measured value of the melting point of the slag without volatile components, and the difference value of the melting points of the two slag corresponding to the same heating rate is the influence of the volatilization of the slag on the melting point of the slag; subtracting the value of the elevation affected by volatilization from the measured value of the melting point of the slag containing the volatile components to obtain the melting point not affected by volatilization, and then extrapolating out to obtain the theoretical value of the melting point of the slag containing the volatile components when the temperature rising rate is 0. Fully considers the influence of slag volatile components on the melting point, and obtains more accurate melting point.
Description
Technical Field
The invention belongs to the field of metallurgical engineering, and particularly relates to an evaluation method for the influence of slag volatilization containing volatile components on a melting point.
Background
Pyrometallurgy is the main preparation method of bulk metals, the steel yield in 2020 reaches 10.53 hundred million tons, the nonferrous metal lead yield reaches 664.3 ten thousand tons, the zinc yield reaches 642.5 ten thousand tons, and the nonferrous metal lead zinc yield reaches 1306.8 ten thousand tons. Pyrometallurgical processes involve a large number of different metallurgical melts including metal melts, molten slag, molten matte, molten salt, and the like. The composition and physical and chemical properties of the melt are not only important references for controlling the metallurgical process. Taking metallurgical slag as an example, the components and the physical and chemical properties of the metallurgical slag are closely related to the temperature control, interface reaction characteristics, inclusion removal and even the forward running of the smelting process. Slag properties mainly include melting point, viscosity, crystallization properties, surface tension, etc., wherein melting point is the most critical parameter in the control of properties.
If the slag contains volatile components, when the traditional method is used for measuring the melting point, the temperature rise and the heat preservation usually need a plurality of hours, so that a large amount of volatile components in the slag volatilize, and according to the related measurement, the fluoride volatilization amount in part of ferrous metallurgical slag can reach more than 30 percent; the volatilization rate of lead and the compounds thereof can reach more than 40 percent, and the volatilization rate converted into volatile components is more striking. From this, it is clear that the effect of such volatilization on slag composition and properties is quite obvious. Under the high temperature condition, the volatile components can be volatilized continuously, so that the slag components are changed continuously, further, the physical parameters of the slag are changed, and finally, the accurate slag melting temperature, namely the so-called slag melting temperature 'inaccurate' cannot be obtained. Metallurgical melts with high-temperature volatilization are of various types, and typically comprise alkali metal alkaline earth metals and alloys thereof, lead-zinc-cadmium and the like and alloys thereof, high-manganese alloys, lead-zinc and alloys thereof, lead-zinc slag, fluoride-containing and potassium-sodium-oxygen slag, molten salt, phosphorus-arsenic-rich slag and the like. In addition, in some specialty metallurgies, the problem of volatilization is also pronounced due to the very high temperatures, and the same problem is faced in determining the performance of the alloy Jin Gaowen. Therefore, the problem is a common basic theory problem to be solved, which has wide related fields and wide influence range. In the volatile pyrometallurgical slag, the ferrous metal smelting process is particularly remarkable with the fluorine-containing slag; the volatile components of lead-zinc smelting slag are most obvious in the nonferrous metal smelting process. Thus, the melting point determination of this type of slag cannot be accommodated using conventional methods.
Disclosure of Invention
The invention aims to provide an evaluation method for the influence of volatilization of slag containing volatile components on a melting point, so as to solve the technical problem of inaccurate melting point measurement caused by using slag containing volatile components in the pyrometallurgical process, thereby obtaining a more accurate melting point and providing support for controlling and optimizing the pyrometallurgical process involving slag containing volatile components.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for evaluating the influence of slag volatilization containing volatile components on a melting point comprises the following steps:
measuring the melting point of the same slag containing the volatile components under different heating rates to obtain a corresponding relation curve of the melting point of the slag containing the volatile components and the heating rate;
measuring the melting points of the same non-volatile component slag at different heating rates to obtain a corresponding relation curve of the melting points of the non-volatile component slag and the heating rates;
when the heating rate is extrapolated to 0 according to the corresponding relation curve of the melting point of the non-volatile component slag and the heating rate, obtaining a measured value of the melting point of the non-volatile slag, wherein the heating rate tends to be zero;
when the heating rate is extrapolated to 0 according to the corresponding relation curve of the melting point of the slag containing the volatile components and the heating rate, obtaining a measurement value of the melting point of the volatile slag with the heating rate tending to zero;
the corresponding relation curve of the melting point of the non-volatile component slag and the heating rate is downwards moved to the state that the measured value of the melting point of the non-volatile slag is overlapped with the measured value of the melting point of the volatile slag, and the difference value of the melting points of the two slag corresponding to the same heating rate is the influence value of the volatilization of the slag on the melting point of the slag;
subtracting the influence value of slag volatilization on the slag melting point from the melting point of the slag containing the volatile components and the corresponding relation curve of the heating rate to obtain the corresponding relation curve of the melting point which is not influenced by volatilization and the heating rate, and extrapolating out the heating rate to be 0 to obtain the theoretical melting point value of the slag containing the volatile components.
The invention further improves that: when the correspondence between the slag melting point and the temperature rising rate is measured, a hemispherical melting point measurement method is adopted.
The invention further improves that: when the correspondence between the slag melting point and the temperature rising rate is measured, one of differential thermal analysis, ash melting point measurement or taper sample measurement is adopted.
The invention further improves that: the temperature rising rate is in the range of 5-30 ℃/min.
The invention further improves that: the temperature rising rate is within the range of 5-30 ℃/min, and 4 or more than 4 temperature rising rate values are taken for temperature rising.
The invention further improves that: the heating rate is 30 ℃/min or 35 ℃/min at the maximum.
The invention further improves that: and weighing samples of the slag to be tested before and after measuring all the melting points to obtain the content change of volatile components in the slag, and evaluating the influence of the volatile components in the slag on the melting point of the slag according to the content change of the volatile components in the slag and the influence value of the slag volatilization on the melting point of the slag.
The invention further improves that: when the slag to be measured is subjected to sample weighing, a balance with the measurement precision of more than or equal to 0.0001g is adopted.
The invention further improves that: when the melting point of the slag containing the volatile components with high volatility is measured, the heating rate is improved.
Compared with the prior art, the invention has at least the following beneficial effects:
1. the influence of the slag volatile components on the melting point of the slag is fully considered, so that a more accurate melting point is obtained, and the influence of the slag volatile components on the melting point is measured and evaluated.
2. The existing measuring device and measuring method for the melting point of the slag containing the volatile components for pyrometallurgy can be utilized, the existing related measuring results can be utilized to the maximum extent, and the measuring difficulty is reduced.
3. And evaluating the influence of the slag containing volatile components on the melting point of the slag, and processing the measured melting point of the slag according to an evaluation result to obtain a more accurate theoretical melting point value.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 is a schematic diagram of slag determination using hemispherical melting point determination;
FIG. 2 is a schematic diagram of an evaluation of the effect of temperature-reflected hysteresis and slag formation on melting point in the steelmaking of fluorine-free slag and fluorine-containing slag;
FIG. 3 is a schematic view of the evaluation of the effect of volatile components in slag on melting point during steelmaking with fluorine-free slag and fluorine-containing slag;
FIG. 4 is a schematic diagram for measuring and calculating the theoretical melting point value of slag after volatilization of fluorine-free slag and fluorine-containing slag during steelmaking.
Detailed Description
The invention will be described in detail below with reference to the drawings in connection with embodiments. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The following detailed description is exemplary and is intended to provide further details of the invention. Unless defined otherwise, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the invention.
The invention relates to a method for evaluating the influence of slag volatilization containing volatile components on a melting point, which comprises the following steps:
when the melting point of slag, namely the melting temperature is measured, a hemispherical point melting point measuring method is adopted, namely, the slag containing volatile components for pyrometallurgy is prepared according to the component requirement, a columnar sample is pressed, dried and then is put into a measuring device, and then the temperature is continuously increased according to a certain heating rate, so that the shape change of the sample is observed. As shown in FIG. 1, for example, CQKJ-II type slag melting temperature characteristic measuring instrument is used, a cylindrical sample of 3X 3mm is used, and the temperature is slowly raised at a set rate (5 to 30 ℃ C./min). When the height of the sample is reduced by 1/6, the corresponding temperature of the sample projection corner is used as the initial melting temperature when the sample projection corner begins to be rounded; when the height of the sample is reduced by half and the projection profile on the sample is approximately hemispherical, the corresponding temperature is called hemispherical temperature or melting temperature, hereinafter, the hemispherical temperature is called as melting point, and the height is reduced to 1/3 or 1/4 of the original sample height, which is called as complete melting temperature or flow temperature.
The basic measurement method comprises the following steps: determination the basic method of conventional metallurgical slag melting point YB/T186-2014 "determination of slag melting point" is still adopted, but the rate of temperature rise needs to be changed and the determination of the melting point of the same and volatile slag needs to be carried out for the non-volatile component slag. Other melting point determination methods, such as differential thermal analysis, ash melting point determination methods, cone-shaped sample (refractory cone) determination methods, and the like, may also be used.
The step of changing the temperature rising rate comprises the following steps:
and in the heating rate range of 5-30 ℃/min, adopting a conventional hemispherical slag melting point measuring method to measure the melting points of the same slag sample at different heating rates respectively, and obtaining corresponding relation curves of the melting points and the heating rates, wherein the curves are shown as a curve 2 and a curve 3 in fig. 2. In order to make extrapolation more accurate, the heating rate should be at least 4 points, and the maximum heating rate should be 30 ℃/min or 35 ℃/min. In the measuring process, respectively weighing and measuring slag samples before and after measurement;
there is a difference in volatility due to slag containing volatile components. For slag with strong volatility, low heating rate means long duration of a high temperature section and large volatilization amount. Therefore, the heating rate needs to be appropriately increased for the slag having high volatility.
For example, at a heating rate of 5 ℃ per minute to 15 ℃ per minute, the highly volatile slag is completely volatilized. The melting point of the slag is very similar when measured; at a heating rate of 20 ℃/min, the slag is not completely volatilized, and the melting point difference occurs. Therefore, in measuring the melting point of slag having high volatility, the rate of temperature rise is appropriately increased.
The melting point determination step of the non-volatile component slag comprises the following steps:
selecting a group of slag without volatile components, preparing the granularity of slag materials and the like to be consistent with the slag with volatile components as far as possible, and adopting a conventional hemispherical metallurgical slag melting point measuring method within the temperature rising rate range of 5-30 ℃/min to respectively measure the melting points at different temperature rising rates to obtain a corresponding relation curve of the melting points and the temperature rising rates, wherein the curve 2 is shown in figure 2. In order to make extrapolation more accurate, the heating rate should be not less than 4 points, and the maximum heating rate should be not less than 30 ℃/min. In the measurement process, the slag samples before and after the measurement are weighed and measured.
The measurement process temperature reflects the evaluation of the comprehensive influences of hysteresis, slag formation, melting and the like: the resulting curve 2 of FIG. 2 is extrapolated to a zero heating rate, resulting in a melting point measurement where the heating rate tends to zero, which is an infinitely small slag heating rate, i.e., one without a measured process temperature lag. With this value as horizontal line 1, the shaded area between line 1 and curve 2 is the effect of the temperature hysteresis of the slag melting point determination process. Taking the temperature rising rate of 25 ℃/min as an example, the temperature difference corresponding to the line segment AB is the temperature rising rate of 25 ℃/min, and the melting point measurement deviation value is caused by temperature reflection lag. For the same slag sample, as the temperature rising rate increases, the melting point measurement value increases, and the measurement result becomes higher due to the separate melting. Therefore, the influence of the temperature reflection lag, the melting point, and the like in the measurement process can be evaluated by using the plotted curve 2 and the straight line 1. If the influence of the temperature-reflected hysteresis is subtracted from the measured melting point value, the theoretical melting point value of the non-volatile slag, which does not change with the change in the temperature rise rate, can be obtained.
Evaluation of volatilization influence: the curve 3 in fig. 2 is extrapolated to obtain a point D, which is a melting point measurement value when the temperature rising rate of the volatile slag approaches infinity, and this point can reflect the melting point measurement value obtained by the volatile slag after the volatile slag is fully volatilized, and the actual composition of the slag at this time has changed significantly, while the other points in the curve 3 reflect the results of the combined actions of slag volatilization, temperature reflection lag, slag melting and the like. The curve 2 and the line 1 are translated together so that their point at which the temperature tends to zero coincides with the point D, giving the result shown in figure 3. The shaded part between the curve 2 and the straight line 3 after translation can show that the volatile slag temperature reflects the influence of hysteresis and partial melting, the similar substances are considered to be adopted for preparing slag, the granularity, the compaction degree and the like are the same, and the hysteresis equivalent of the measuring process is basically consistent. The distance between curve 3 and curve 2 reflects the effect of volatilization on the measurement result, namely, the effect of considering "hysteresis + melting by division" is curve 2, the effect of considering "volatilization + hysteresis + melting by division" is curve 1, and the difference between the two is the effect of "volatilization". Also taking a heating rate of 25 ℃/min as an example, the temperature difference corresponding to the line segment AB is the change of the melting point measured value due to temperature reflection lag and partial melting, and the temperature difference corresponding to the line segment AC is the change of the melting point measured value due to volatilization, wherein the heating rate is 25 ℃/min.
Measurement of theoretical melting point: since the reduction of the zero volatilization is caused by the reduction of the residence time at high temperature in view of volatilization, that is, due to the increase of the heating rate, the value of the decrease of the melting point measurement value is the corresponding value of the line segment AC, if the melting point measurement value effective to suppress the volatilization of slag is the melting point measurement value of the line segment AC, the corresponding point on the curve 3 should be compensated for to some extent, and the result of the volatilization influence is the result of the downward movement of the corresponding point, that is, the result shown in the curve 4. That is, the slower the temperature rise rate, the more volatile and the more compensation. The heating rate is about 30 ℃/min, the distance between the curve 2 and the curve 3 is basically unchanged, that is to say, the volatilization effect at the point is basically zero, and no compensation is needed at the moment. The lower the rate of temperature rise, the more compensation. For this purpose, the influence line such as temperature response lag in fig. 3 is shifted down to align with the point E in fig. 4 (that is, this point is not compensated). Taking the heating rate of 5 ℃/min as an example, if volatilization can be effectively inhibited, the apparent measurement value of the melting point is a corresponding value of the point H, but the melting point is increased due to volatilization of volatile components, the melting point value measured by adopting a conventional hemispherical steelmaking slag melting point measuring method is the point G, obvious deviation occurs between the two points, and the line segment GH is the deviation, namely the compensation value which should be given. Further, if the influence of hysteresis is removed from the temperature, the melting point should be the point corresponding to the straight line of the graph, that is, the temperature corresponding to the point F, which should be the theoretical melting point corresponding to the slag (original composition), volatilization is suppressed, and there is no hysteresis in the reaction temperature. The melting point value does not change with the change of the temperature rising rate and the volatilization of the components.
(5) Evaluation of the amount of volatilization: the slag sample is weighed before and after the melting point measurement, the content change of volatile components in the slag can be estimated, and the influence of the volatile components in the slag on the melting point of the slag is evaluated according to the content change of the volatile components in the slag and the influence value of the slag volatilization on the melting point of the slag. In order to ensure accurate weighing, more than one ten thousandth of precision balance should be adopted.
The following are specific application examples:
example 1
Evaluation of influence of volatilization in determination of melting point of fluorine slag in electroslag remelting and correction of result
Slag and conventional melting point determination are selected
The composition of the medium fluorine slag and slag for electroslag remelting is shown in table 1. The slag is mixed slag prepared by chemical pure reagent.
TABLE 1 slag component (wt/%) of medium fluorine slag for electroslag remelting
| Slag of furnace | Al 2 O3 | MgO | SiO 2 | CaF 2 | CaO |
| Middle fluorine slag | 29.33 | 2.57 | 9.15 | 30.12 | 28.83 |
| Fluorine-free slag | 18 | - | 42 | - | 40 |
And measuring by adopting hemispherical points, wherein the heating rate is 10 ℃/min, and measuring to obtain the hemispherical points of the medium fluorine slag at 1351 ℃ and the corresponding melting point of the fluorine-free slag at 1432 ℃.
Application mode
According to the method, 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and 30 ℃/min are adopted to measure the hemispherical temperature of two kinds of slag, a curve of the change of the melting point along with the heating rate is drawn, and the comprehensive influence values of the fluorine-free slag such as 'temperature + slag forming reaction + melting separation' and the like and the influence values of the fluorine-free slag such as 'temperature + slag forming reaction + melting separation' and 'volatilization influence' are obtained respectively through coupling and extrapolation. And further extrapolated to obtain melting point theoretical values of the medium fluorine slag and the fluorine-free slag.
Application results
According to the method, when the comprehensive influence values such as temperature, slag forming reaction, separate melting and the like are obtained and gradually increased to 30 ℃ per minute along with the heating rate, the apparent melting point value obtained by measuring the fluorine-free slag is gradually increased to 1501 ℃ from 1432 ℃; the apparent melting point value obtained by measuring the middle slag is gradually reduced from 1380 ℃ to 1288 ℃, and the maximum influence of volatilization can reach 212 ℃. Further correction results in a melting point theoretical value of 1225 ℃ for the medium fluorine slag, which is basically close to the measured value 1240 ℃ of the premelted slag (the volatilization of the premelted slag is far less than that of the mixed slag) with the same chemical composition, and the credibility of the premelted slag is proved.
Example 2
Evaluation of volatile influence in determination of melting point of high-fluorine slag for electroslag remelting and correction of result
Slag and conventional melting point determination are selected
The composition of the high-fluorine slag for electroslag remelting and the slag composition are shown in table 2, and the slag is mixed slag prepared by chemical pure reagents.
TABLE 2 slag component (wt/%) of high-fluorine slag melting point for electroslag remelting
| Slag of furnace | Al 2 O 3 | SiO 2 | CaF 2 | CaO |
| High fluorine slag | 28.89 | 2.99 | 68.12 | - |
| Fluorine-free slag | 18 | 42 | - | 40 |
And measuring by adopting hemispherical points, wherein the heating rate is 10 ℃/min, and measuring to obtain the hemispherical points of the high fluorine slag at 1351 ℃ and the corresponding melting points of the fluorine-free slag at 1432 ℃.
Application mode
According to the method, 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and 30 ℃/min are adopted to measure the hemispherical temperature of two kinds of slag, a curve of the change of the melting point along with the heating rate is drawn, and the comprehensive influence values of the fluorine-free slag such as 'temperature + slag forming reaction + melting separation' and the like and the influence values of the fluorine-free slag such as 'temperature + slag forming reaction + melting separation' and 'volatilization influence' are obtained respectively through coupling and extrapolation. And further extrapolated to obtain melting point theoretical values of the medium fluorine slag and the fluorine-free slag.
Application results
According to the method, when the comprehensive influence values such as temperature, slag forming reaction, separate melting and the like are obtained and gradually increased to 30 ℃ per minute along with the heating rate, the apparent melting point value obtained by measuring the fluorine-free slag is gradually increased to 1501 ℃ from 1432 ℃; the apparent melting point value obtained by measuring the middle slag is gradually reduced from 1351 ℃ to 1270 ℃, and the maximum influence of volatilization can reach 81 ℃. Further correction is carried out to obtain the theoretical melting point value of the high-fluorine slag which is 1201 ℃.
Example 3
Evaluation of influence of volatilization in melting point measurement of fluorine-containing casting powder for steelmaking and result correction
Slag and conventional melting point determination are selected
Two continuous casting mold flux with the same chemical composition, wherein one is mixed slag prepared by adopting chemical pure reagent, and the other is premelted slag (after carbon removal). The composition of the slag is shown in table 3,
TABLE 3 slag component (wt/%) of fluorine-containing protective slag for steelmaking
And measuring by adopting a hemispherical point, wherein the heating rate is 10 ℃/min, and the hemispherical point temperature of the mixed slag of the fluorine-containing covering slag is 1125 ℃ and the corresponding hemispherical point temperature of the premelted slag is 1032 ℃. The melting point of the fluorine-free covering slag is 1170 ℃.
Application mode
According to the method, 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and 30 ℃/min are adopted to measure the hemispherical temperature of three slags, a curve of the change of the melting point along with the heating rate is drawn, and the comprehensive influence values of 'temperature + slagging reaction + melting separation' of the fluorine-free covering slag and the like and the corresponding influence values of 'temperature + slagging reaction + melting separation' and 'volatilization influence' of the fluorine-containing slag are obtained respectively through coupling and extrapolation. And further extrapolated to obtain the theoretical melting point value of the mixed slag of the fluorine-containing protecting slag, and comparing the theoretical melting point value with the melting point measurement result of the premelted slag of the fluorine-containing slag.
Application results
According to the method, when the comprehensive influence values such as temperature, slag forming reaction, separate melting and the like are obtained and gradually increased to 30 ℃ per minute from 5 ℃ per minute along with the heating rate, the apparent melting point value obtained by measuring the fluorine-free covering slag is gradually increased to 1211 ℃ from 1170 ℃; the apparent melting point value obtained by measuring the fluorine-containing mixed slag is gradually reduced from 1125 ℃ to 1061 ℃, so that the maximum influence of volatilization can reach about 64 ℃. The melting point theoretical value of the mixed slag of the fluorine-containing covering slag obtained by further correction is 1020 ℃, and the melting point theoretical value is basically close to the measured value 1032 ℃ of the premelting slag (the volatilization of the premelting slag is far smaller than that of the mixed slag) adopting the same chemical composition, thus proving the credibility.
Example 4 evaluation of the Effect of volatilization in melting Point measurement of lead slag in lead direct reduction and correction of the result
Slag and conventional melting temperature measurement are selected
The composition of the lead slag in the direct reduction of lead is shown in Table 4. The slag is mixed slag prepared by chemical pure reagent.
TABLE 4 slag content of lead slag in lead direct reduction (wt/%)
| Composition of the components | PbO | ZnO | CaO | FeO | SiO 2 |
| Lead slag in the middle | 20 | 10 | 12.35 | 37.06 | 20.59 |
| Lead free slag | - | 12.50 | 15.44 | 46.33 | 25.74 |
And measuring by adopting a hemispherical point, wherein the heating rate is 10 ℃/min, and measuring to obtain the hemispherical melting temperature of the medium lead slag of 1226 ℃ and the corresponding melting temperature of the lead-free slag of 1292 ℃.
Application mode
According to the method, 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and 30 ℃/min are adopted to measure the hemispherical temperature of two kinds of slag, a change curve of the melting temperature along with the heating rate is drawn, comprehensive influence values such as 'temperature + slagging reaction + partial melting' of lead-free slag and the like are respectively obtained through coupling and extrapolation, and influence values corresponding to 'temperature + slagging reaction + partial melting' and 'volatilization influence' of the lead-free slag are respectively obtained, so that influence evaluation on volatilization and other factors can be realized, and further the theoretical melting temperature values of the lead-free slag and the lead-free slag are extrapolated.
Application results
According to the method, when the comprehensive influence values such as temperature, slag forming reaction, separate melting and the like are obtained and gradually increased to 30 ℃ per minute from 5 ℃ per minute along with the heating rate, the apparent melting temperature value obtained by measuring the lead-free slag is gradually increased to 1359 ℃ from 1286 ℃; the apparent melting temperature value obtained by measuring the lead slag is gradually reduced from 1263 ℃ to 1151 ℃, and the maximum volatilization influence can reach 208 ℃. The theoretical melting temperature of the lead slag obtained by further correction is 1075 ℃, which is basically close to the measured value 1056 ℃ of the premelted slag (the volatilization of the premelted slag is far less than that of the mixed slag) adopting the same chemical composition, and the credibility of the premelted slag is proved.
Example 5
Evaluation of influence of volatilization in melting point measurement of high lead slag in direct reduction of lead and correction of result
Slag and conventional melting temperature measurement are selected
The composition of the medium-high lead slag in the direct reduction is shown in Table 5. The slag is mixed slag prepared by chemical pure reagent.
TABLE 5 slag content (wt/%) of medium-high lead slag in direct reduction of lead
| Composition of the components | PbO | ZnO | CaO | FeO | SiO 2 |
| Lead slag in the middle | 40 | 6 | 9.53 | 28.58 | 15.88 |
| Lead free slag | - | 10.00 | 15.88 | 47.63 | 26.47 |
And measuring by adopting a hemispherical point, wherein the heating rate is 10 ℃/min, and the measuring result shows that the hemispherical melting temperature of the high lead slag is 1206 ℃ and the corresponding melting temperature of the lead-free slag is 1296 ℃.
Application mode
According to the method, 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min, 30 ℃/min and the like are respectively adopted to measure the hemispherical temperature of two kinds of slag, a change curve of the melting temperature along with the heating rates is drawn, and the comprehensive influence values of 'temperature + slagging reaction + partial melting' and the like of lead-free slag and the influence values of 'temperature + slagging reaction + partial melting' and 'volatilization influence' of corresponding lead slag are respectively obtained through coupling and extrapolation, so that the influence evaluation on volatilization and other factors can be realized, and further the theoretical melting temperature values of the lead slag and the lead-free slag are extrapolated.
Application results
According to the method, when the comprehensive influence values such as temperature, slag forming reaction, separate melting and the like are obtained and gradually increased to 30 ℃ per minute from 5 ℃ per minute along with the heating rate, the apparent melting temperature value obtained by measuring the lead-free slag is gradually increased to 1364 ℃ from 1291 ℃; the apparent melting temperature value obtained by the measurement of the medium lead slag is gradually reduced from 1261 ℃ to 1130 ℃, and the maximum influence of volatilization can reach 234 ℃. The theoretical melting temperature of the lead slag obtained by further correction is 1053 ℃, which is basically close to the measured value 1020 ℃ of the premelting slag (the volatilization of the premelting slag is far less than that of the mixed slag) with the same chemical composition, thus proving the credibility.
Example 6
Evaluation of influence of volatilization in melting point measurement of high lead slag in initial stage of direct reduction of lead and correction of result
Slag and conventional melting temperature measurement are selected
The composition of the blast-furnace slag in the initial stage of the direct reduction is shown in Table 6. The slag is mixed slag prepared by chemical pure reagent.
TABLE 6 slag content (wt/%) of high lead slag in the initial stage of lead direct reduction
| Composition of the components | PbO | ZnO | CaO | FeO | SiO 2 |
| Lead slag in the middle | 61.26 | 9.17 | 3.48 | 19.99 | 5.26 |
| Lead free slag | - | 24.20 | 9.18 | 52.74 | 13.88 |
And measuring by adopting a hemispherical point, wherein the heating rate is 10 ℃/min, and measuring to obtain the hemispherical melting temperature of the high lead slag of 1113 ℃ and the corresponding melting temperature of the lead-free slag of 1215 ℃.
Application mode
According to the method, 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min, 30 ℃/min and the like are respectively adopted to measure the hemispherical temperature of two kinds of slag, a change curve of the melting temperature along with the heating rates is drawn, and the comprehensive influence values of 'temperature + slagging reaction + partial melting' and the like of lead-free slag and the influence values of 'temperature + slagging reaction + partial melting' and 'volatilization influence' of corresponding lead slag are respectively obtained through coupling and extrapolation, so that the influence evaluation on volatilization and other factors can be realized, and further the theoretical melting temperature values of the lead slag and the lead-free slag are extrapolated.
Application results
According to the method, when the comprehensive influence values such as temperature, slag forming reaction, partial melting and the like are obtained and gradually increased to 30 ℃ per minute along with the heating rate, the apparent melting temperature value obtained by measuring the lead-free slag is gradually increased to 1314 ℃ from 1205 ℃; the apparent melting temperature value obtained by measuring the high lead slag is gradually reduced from 1168 ℃ to 955 ℃, and the influence of volatilization can reach 359 ℃ at maximum. The theoretical melting temperature of the high lead slag obtained by further correction is 842 ℃, which is basically close to the measured value 812 ℃ of the premelting slag (the volatilization of the premelting slag is far less than that of the mixed slag) adopting the same chemical composition, thus proving the credibility.
It will be appreciated by those skilled in the art that the present invention can be carried out in other embodiments without departing from the spirit or essential characteristics thereof. Accordingly, the above disclosed embodiments are illustrative in all respects, and not exclusive. All changes that come within the scope of the invention or equivalents thereto are intended to be embraced therein.
Finally, it should be noted that: the above embodiments are only for illustrating the technical aspects of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those of ordinary skill in the art that: modifications and equivalents may be made to the specific embodiments of the invention without departing from the spirit and scope of the invention, which is intended to be covered by the claims.
Claims (6)
1. A method for evaluating the effect of volatilization of slag containing volatile components on a melting point, which is characterized by comprising the following steps:
measuring the melting point of the same slag containing the volatile components under different heating rates to obtain a corresponding relation curve of the melting point of the slag containing the volatile components and the heating rate;
measuring the melting points of the same non-volatile component slag at different heating rates to obtain a corresponding relation curve of the melting points of the non-volatile component slag and the heating rates;
when the heating rate is extrapolated to 0 according to the corresponding relation curve of the melting point of the non-volatile component slag and the heating rate, obtaining a measured value of the melting point of the non-volatile slag, wherein the heating rate tends to be zero;
when the heating rate is extrapolated to 0 according to the corresponding relation curve of the melting point of the slag containing the volatile components and the heating rate, obtaining a measurement value of the melting point of the volatile slag with the heating rate tending to zero;
the corresponding relation curve of the melting point of the non-volatile component slag and the heating rate is downwards moved to the state that the measured value of the melting point of the non-volatile slag is overlapped with the measured value of the melting point of the volatile slag, and the difference value of the melting points of the two slag corresponding to the same heating rate is the influence value of the volatilization of the slag on the melting point of the slag;
subtracting the influence value of slag volatilization on the slag melting point from the melting point of the slag containing the volatile components and the corresponding relation curve of the heating rate to obtain a corresponding relation curve of the melting point which is not influenced by volatilization and the heating rate, and extrapolating out the heating rate to be 0 to obtain the theoretical melting point value of the slag containing the volatile components;
weighing samples of the slag to be tested before and after measuring all the melting points to obtain the content change of volatile components in the slag, and evaluating the influence of the volatile components in the slag on the melting point of the slag according to the content change of the volatile components in the slag and the influence value of the slag volatilization on the melting point of the slag;
when the slag to be measured is subjected to sample weighing, a balance with the measurement precision of more than or equal to 0.0001g is adopted;
when the melting point of the slag containing the volatile components with high volatility is measured, the heating rate is improved.
2. The method for evaluating the influence of volatilization of slag containing a volatile component on a melting point according to claim 1, wherein a hemispherical melting point measurement method is used when the correspondence between the melting point of slag and the rate of temperature rise is measured.
3. The method for evaluating the effect of volatilization of slag containing a volatile component on a melting point according to claim 1, wherein one of differential thermal analysis, ash melting point measurement or taper sample measurement is used in measuring the correspondence between the melting point of slag and the rate of temperature rise.
4. The method for evaluating the influence of volatilization of slag containing volatile components on a melting point according to claim 1, wherein the heating rate is in the range of 5-30 ℃/min.
5. The method for evaluating the influence of volatilization of slag containing volatile components on a melting point according to claim 4, wherein the heating rate is in the range of 5-30 ℃/min, and 4 or more heating rate values are used for heating.
6. The method for evaluating the effect of volatilization of slag containing volatile components on melting point according to claim 1, wherein the heating rate is at most 30 ℃/min or 35 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111417614.6A CN114137017B (en) | 2021-11-25 | 2021-11-25 | Evaluation method for influence of slag volatilization containing volatile components on melting point |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111417614.6A CN114137017B (en) | 2021-11-25 | 2021-11-25 | Evaluation method for influence of slag volatilization containing volatile components on melting point |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114137017A CN114137017A (en) | 2022-03-04 |
| CN114137017B true CN114137017B (en) | 2024-01-23 |
Family
ID=80388284
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111417614.6A Active CN114137017B (en) | 2021-11-25 | 2021-11-25 | Evaluation method for influence of slag volatilization containing volatile components on melting point |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114137017B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH472030A (en) * | 1966-05-23 | 1969-04-30 | Meehanite Metal Corp | Process for determining the iron oxide content in slag and application of this process for setting the degree of oxidation during a metal smelting process |
| CN1623003A (en) * | 2000-08-09 | 2005-06-01 | 株式会社神户制钢所 | Method for producing metallic iron |
| RU2441080C1 (en) * | 2010-07-29 | 2012-01-27 | Закрытое акционерное общество "Управляющая компания "НКА-Холдинг" | Method of producing copper matte |
| CN105445138A (en) * | 2015-11-27 | 2016-03-30 | 西安建筑科技大学 | Slag actual ingredient performance detection method for slag containing volatile components |
| CN109541143A (en) * | 2018-11-28 | 2019-03-29 | 西安建筑科技大学 | A kind of prediction technique that the constituent element clinker actual constituent transitivity containing volatilization changes over time |
-
2021
- 2021-11-25 CN CN202111417614.6A patent/CN114137017B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH472030A (en) * | 1966-05-23 | 1969-04-30 | Meehanite Metal Corp | Process for determining the iron oxide content in slag and application of this process for setting the degree of oxidation during a metal smelting process |
| CN1623003A (en) * | 2000-08-09 | 2005-06-01 | 株式会社神户制钢所 | Method for producing metallic iron |
| RU2441080C1 (en) * | 2010-07-29 | 2012-01-27 | Закрытое акционерное общество "Управляющая компания "НКА-Холдинг" | Method of producing copper matte |
| CN105445138A (en) * | 2015-11-27 | 2016-03-30 | 西安建筑科技大学 | Slag actual ingredient performance detection method for slag containing volatile components |
| CN109541143A (en) * | 2018-11-28 | 2019-03-29 | 西安建筑科技大学 | A kind of prediction technique that the constituent element clinker actual constituent transitivity containing volatilization changes over time |
Non-Patent Citations (1)
| Title |
|---|
| 升温速率与预熔过程对含氟渣熔点影响分析;赵忠宇;赵俊学;谭泽馨;屈波樵;卢亮;崔雅茹;;钢铁(第06期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114137017A (en) | 2022-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xu et al. | Effect of Al2O3 on the viscosity of CaO-SiO2-Al2O3-MgO-Cr2O3 slags | |
| CN110172648B (en) | Zirconium-containing electrothermal alloy and preparation method of zirconium-containing alloy | |
| CN105838846A (en) | Method for controlling basicity of LF refining slag | |
| Shiau et al. | Effect of magnesium and aluminum oxides on fluidity of final blast furnace slag and its application | |
| CN114137017B (en) | Evaluation method for influence of slag volatilization containing volatile components on melting point | |
| CN104388612B (en) | A kind of blast furnace low cost titanium ore furnace retaining method | |
| CN111440916B (en) | Method for producing ultra-low manganese steel by using high-manganese molten iron converter | |
| JP4486878B2 (en) | Mold powder for continuous casting of steel and continuous casting method | |
| KR101185300B1 (en) | Method for estimating position bordered to furnace wall of softening zone | |
| CN107245636B (en) | A kind of smelting pouring procedure of same heat different chemical composition alloy | |
| JP2926449B2 (en) | Kiln operation and refractory lining | |
| JP7211550B2 (en) | Molten metal desulfurization method | |
| Shiau et al. | Effect of magnesium oxide content on final slag fluidity of blast furnace | |
| TWI729791B (en) | Method for improving slag liquidity | |
| JPH0954057A (en) | Consumptive electric conductivity measuring probe and method for measuring electric conductivity of molten oxide | |
| CN102146521A (en) | Method for reducing stannum content of liquid copper in shaft furnace for regenerating and refining recycled copper | |
| Tan et al. | Modelling of slag blow in copper Peirce-Smith Converters | |
| Shiau | Real-time indices focus on slag flowability and coke strength for blast furnace operation | |
| JPH06341773A (en) | Operation stabilizing method for electric furnace | |
| CN114269705A (en) | Low-melting tin phosphate glass frit | |
| Tan | Applications of thermo-chemical and thermo-physical modeling in the copper converter industries' | |
| Mei et al. | Real-Time Carbon and Temperature Model of Converter Based on the Weights of Elemental Reaction Rate | |
| JPH048483B2 (en) | ||
| CN116590493A (en) | Antimony adding method for improving antimony yield in steelmaking process | |
| JPS6256512A (en) | Method for controlling converter blowing |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |