CN114137017A - Method for evaluating influence of volatilization of slag containing volatile components on melting point - Google Patents
Method for evaluating influence of volatilization of slag containing volatile components on melting point Download PDFInfo
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- CN114137017A CN114137017A CN202111417614.6A CN202111417614A CN114137017A CN 114137017 A CN114137017 A CN 114137017A CN 202111417614 A CN202111417614 A CN 202111417614A CN 114137017 A CN114137017 A CN 114137017A
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- 239000002893 slag Substances 0.000 title claims abstract description 295
- 238000002844 melting Methods 0.000 title claims abstract description 221
- 230000008018 melting Effects 0.000 title claims abstract description 221
- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000010438 heat treatment Methods 0.000 claims abstract description 52
- 238000005259 measurement Methods 0.000 claims description 44
- 230000000630 rising effect Effects 0.000 claims description 19
- 230000008859 change Effects 0.000 claims description 17
- 238000005303 weighing Methods 0.000 claims description 5
- 238000004455 differential thermal analysis Methods 0.000 claims description 3
- 239000011133 lead Substances 0.000 description 34
- 229910052731 fluorine Inorganic materials 0.000 description 29
- 239000011737 fluorine Substances 0.000 description 29
- 239000000203 mixture Substances 0.000 description 25
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 24
- 238000006243 chemical reaction Methods 0.000 description 22
- 238000011156 evaluation Methods 0.000 description 15
- 239000000126 substance Substances 0.000 description 15
- 238000000926 separation method Methods 0.000 description 13
- 238000012937 correction Methods 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 238000013213 extrapolation Methods 0.000 description 10
- 230000036961 partial effect Effects 0.000 description 10
- 230000002829 reductive effect Effects 0.000 description 10
- 230000008569 process Effects 0.000 description 9
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- 230000008878 coupling Effects 0.000 description 6
- 238000010168 coupling process Methods 0.000 description 6
- 238000005859 coupling reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000009628 steelmaking Methods 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 238000009853 pyrometallurgy Methods 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000914 Mn alloy Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- PIRCGUMCHJTHIE-UHFFFAOYSA-N [O].[Na].[K] Chemical compound [O].[Na].[K] PIRCGUMCHJTHIE-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000001447 compensatory effect Effects 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
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009851 ferrous metallurgy Methods 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
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- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus 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
- 239000010959 steel Substances 0.000 description 1
Images
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 influence of volatilization of slag containing volatile components on a melting point, which comprises the following steps: measuring the melting points of the slag containing the volatile components and the slag without the volatile components at different heating rates to obtain two corresponding relation curves of the melting points and the heating rates; extrapolating according to the two curves to obtain two melting point values when the heating rate is 0; moving a corresponding relation curve of the melting point and the heating rate of the slag without the volatile component downwards to a measured value of the melting point of the slag without the volatile component, wherein the difference of the two melting points of the slag corresponding to the same heating rate is the influence of the volatilization of the slag on the melting point of the slag; and subtracting the value raised by the influence of volatilization from the measured value of the melting point of the slag containing the volatile components to obtain the melting point which is not influenced by volatilization, and then obtaining the theoretical value of the melting point of the slag containing the volatile components when the temperature rise rate is 0. The influence of the slag volatile component on the melting point is fully considered, and a more accurate melting point is obtained.
Description
Technical Field
The invention belongs to the field of metallurgical engineering, and particularly relates to a method for evaluating influence of volatilization of slag containing volatile components on a melting point.
Background
Pyrometallurgy is the main preparation method of bulk metals, the steel yield reaches 10.53 hundred million tons in 2020, the non-ferrous metal lead yield reaches 664.3 ten thousand tons, the zinc yield reaches 642.5 ten thousand tons, and the non-ferrous metal lead-zinc yield reaches 1306.8 ten thousand tons. Pyrometallurgical processes involve a large number of different metallurgical melts including metal melts, molten slags, molten matte, molten salts, and the like. The composition and physical and chemical properties of the melt are not only important basis 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, the interface reaction characteristic, the inclusion removal and even the forward running of the smelting process. Slag properties mainly include melting point, viscosity, crystallization properties, surface tension, etc., where melting point is the most critical parameter in property control.
If the slag contains volatile components, the temperature rise and the heat preservation are usually carried out for several hours when the melting point is measured by using the traditional method, so that a large amount of volatile components in the slag are volatilized, and according to related measurement, the volatilization amount of fluoride in part of the ferrous metallurgy slag can reach more than 30 percent; the volatilization amount of lead and the compound thereof can reach more than 40 percent, and the volatilization rate converted into the volatile component is more surprising. It can be seen that the effect of such volatilization on slag composition and properties is quite significant. Under the condition of high temperature, the volatile components can continuously volatilize, so that the components of the slag are continuously changed, the physical parameters of the slag are changed, and finally, the accurate melting temperature of the slag cannot be obtained, namely the melting temperature of the slag is inaccurate. The metallurgical melt with large high-temperature volatilization amount has various types, and typically comprises alkali metal, alkaline earth metal and alloy thereof, lead, zinc, cadmium and alloy thereof, high manganese alloy, lead, zinc and alloy thereof, lead-containing zinc slag, fluoride-containing potassium-sodium-oxygen slag, molten salt, phosphorus-rich arsenic slag and the like. In addition, in part of special metallurgy, because the temperature is very high, the volatilization problem is obvious, and the same problem can be faced in the measurement of the high-temperature performance of the alloy. Therefore, the problem is a general basic theory problem which is wide in range and wide in influence range and needs to be solved. In volatile pyrometallurgical slag, the smelting process of ferrous metal is particularly remarkable by fluorine-containing slag; the lead-zinc smelting slag has the most obvious volatile component in the non-ferrous metal smelting process. Therefore, the conventional method cannot be applied to the measurement of the melting point of the slag.
Disclosure of Invention
The invention aims to provide a method for evaluating the influence of volatilization of slag containing volatile components on a melting point, which aims to solve the technical problem that the melting point measurement is inaccurate due to the use of the slag containing the volatile components in the pyrometallurgical process, so that a more accurate melting point is obtained, and support is provided for the control and optimization of the pyrometallurgical process of the slag containing the volatile components.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for evaluating the influence of volatilization of slag containing volatile components on a melting point comprises the following steps:
measuring the melting point of the same slag containing the volatile components at different heating rates to obtain a corresponding relation curve of the melting point and the heating rate of the slag containing the volatile components;
measuring the melting point of the same slag without the volatile component at different heating rates to obtain a corresponding relation curve of the melting point of the slag without the volatile component and the heating rate;
extrapolating to obtain a measured value of the melting point of the non-volatile slag with the temperature rising rate tending to zero when the temperature rising rate is 0 according to a corresponding relation curve of the melting point of the non-volatile component slag and the temperature rising rate;
extrapolating to obtain the measured value of the melting point of the volatile slag with the temperature rising rate tending to zero when the temperature rising rate is 0 according to the corresponding relation curve of the melting point of the slag containing the volatile component and the temperature rising rate;
moving a corresponding relation curve of the melting point of the slag without the volatile component and the heating rate downwards to a state that a measured value of the melting point of the slag without the volatile component is coincident with a measured value of the melting point of the volatile slag, wherein the difference value of the two melting points of the slag corresponding to the same heating rate is an influence value of the volatilization of the slag on the melting point of the slag;
and subtracting the influence value of the slag volatilization on the slag melting point from the melting point of the corresponding relation curve of the melting point and the heating rate of the slag containing the volatile component to obtain the corresponding relation curve of the melting point and the heating rate which are not influenced by the volatilization, and then, when the heating rate is 0, obtaining the theoretical value of the melting point of the slag containing the volatile component.
The invention is further improved in that: when the corresponding relation between the slag melting point and the heating rate is measured, a hemispherical point melting point measuring method is adopted.
The invention is further improved in that: when the corresponding relation between the slag melting point and the temperature rise rate is measured, one of differential thermal analysis, ash melting point measurement and cone sample measurement is adopted.
The invention is further improved in that: the temperature rise rate ranges from 5 to 30 ℃/min.
The invention is further improved in that: and the temperature rise rate is within the range of 5-30 ℃/min, and 4 or more than 4 temperature rise rate values are taken for temperature rise.
The invention is further improved in that: the rate of temperature rise is at most 30 ℃/min or 35 ℃/min.
The invention is further improved in that: and (3) weighing the samples of the slag to be measured before and after the measurement of all the melting points to obtain the content change of the volatile components in the slag, and evaluating the influence of the volatilization of the slag containing the volatile components 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 volatilization of the slag on the melting point of the slag.
The invention is further improved in that: and when the sample of the slag to be measured is weighed, a balance with the measurement precision of more than or equal to 0.0001g is adopted.
The invention is further improved in that: when the melting point of the slag containing the volatile components with strong volatility is measured, the heating rate is increased.
Compared with the prior art, the invention has at least the following beneficial effects:
1. the influence of the slag volatile component on the melting point of the slag is fully considered, a more accurate melting point is obtained, and the influence of the slag volatile component on the melting point is measured and evaluated.
2. The existing device and method for determining the melting point of the slag containing the volatile components for pyrometallurgy can be utilized, the existing related determination results can be utilized to the maximum extent, and the measurement difficulty is reduced.
3. And evaluating the influence of the slag containing the volatile components on the melting point of the slag, and processing the measured melting point of the slag according to the evaluation result to obtain a more accurate theoretical value of the melting point.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic illustration of slag determination using hemispherical point melting point measurement;
FIG. 2 is a schematic view showing the evaluation of the influence of temperature reaction lag and slagging on the melting point in the steelmaking process of fluorine-free slag and fluorine-containing slag;
FIG. 3 is a schematic view showing the evaluation of the influence of volatile components in the slag on the melting point in the steelmaking process of the fluorine-free slag and the fluorine-containing slag;
FIG. 4 is a schematic view showing the measurement and calculation of the theoretical melting point of the slag after volatilization during steel making from the fluorine-free slag and the fluorine-containing slag.
Detailed Description
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The following detailed description is exemplary in nature and is intended to provide further details of the invention. Unless otherwise defined, 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 exemplary embodiments according to the invention.
The invention relates to a method for evaluating the influence of volatilization of slag containing volatile components on a melting point, which comprises the following steps:
when the melting point of the slag, namely the melting temperature, is measured, a hemispherical point melting point measuring method is adopted, namely, the slag containing volatile components for pyrometallurgical use is prepared according to the component requirements, a columnar sample is pressed, the columnar sample is placed into a measuring device after being dried, then the temperature is continuously increased according to a certain temperature increasing rate, and the shape change of the sample is observed. As shown in FIG. 1, a CQKJ-II type slag melting temperature characteristic measuring instrument is used as an example, and a cylindrical sample having a diameter of 3X 3mm is used, and the temperature is gradually increased at a set rate (5 to 30 ℃/min). When the height of the sample is reduced 1/6 and the projection corner of the sample begins to round, the corresponding temperature can be used as the initial melting temperature; the corresponding temperature when the height of the sample is reduced by half and the projected profile of the sample is approximately hemispherical is called hemispherical point temperature or melting temperature, hereinafter generically referred to as hemispherical point temperature as melting point, and 1/3 or 1/4 when the height is reduced to the original sample height is called complete melting temperature or flow temperature.
The basic measurement method comprises the following steps: the measurement still adopts the basic method of the conventional metallurgical slag melting point YB/T186-2014 & lt & ltdetermination of slag melting point & gt & lt/EN & gt, but the temperature rising rate needs to be changed and the melting point of the non-volatile component slag and the volatile slag is determined. Other melting point measuring methods, such as differential thermal analysis, ash melting point measuring method, cone sample (refractory cone) measuring method, and the like, may also be used.
The step of varying the rate of temperature rise comprises:
and respectively carrying out melting point measurement on the same slag sample at different heating rates within the heating rate range of 5-30 ℃/min by adopting a conventional semispherical point slag melting point measurement method to obtain a corresponding relation curve of the melting point and the heating rate, as shown in a curve 2 and a curve 3 in fig. 2. In order to make the extrapolation more accurate, the temperature rise rate should be not less than 4 points, and the maximum temperature rise rate should be 30 ℃/min or 35 ℃/min. In the measuring process, respectively weighing and metering the slag samples before and after measurement;
because the volatility of the slag containing the volatile components is different. For slag with strong volatility, the low heating rate means that the high temperature section lasts for a long time and the volatilization amount is large. Therefore, the heating rate needs to be increased appropriately for the volatile strong slag.
For example, at a heating rate of 5 ℃/min to 15 ℃/min, the highly volatile slag is completely volatilized. The melting points of the slag are measured to be very similar; at the temperature rise rate of 20 ℃/min, the slag is not completely volatilized, and the melting point difference occurs. Therefore, when the melting point of slag having high volatility is measured, the temperature increase rate is suitably increased.
The melting point determination step of the non-volatile slag comprises the following steps:
selecting a group of furnace slag without volatile components, preparing furnace slag materials with granularity as consistent as possible with the furnace slag containing the volatile components, and respectively measuring the melting points at different heating rates by adopting a conventional semispherical point metallurgical furnace slag melting point measuring method within the heating rate range of 5-30 ℃/min to obtain a corresponding relation curve of the melting points and the heating rates, wherein the curve is shown as a curve 2 in fig. 2. In order to make the extrapolation more accurate, the temperature rise rate should be not less than 4 points, and the maximum temperature rise rate should be not less than 30 ℃/min. During the measurement, the slag samples before and after the measurement are respectively weighed.
Evaluation of comprehensive influences of temperature reflection lag, slagging, partial melting and the like in the measurement process: extrapolation of the obtained curve 2 in FIG. 2 to a temperature rise rate of zero yields a melting point measurement with a temperature rise rate tending towards zero, which is an infinitesimal slag temperature rise rate, i.e. a melting point measurement without temperature hysteresis in the measurement process. The value is taken as horizontal line 1, and the shaded area between the line 1 and the curve 2 is the influence of the temperature lag in the slag melting point measurement process. Taking the temperature rise rate of 25 ℃/min as an example, the temperature difference corresponding to the line segment AB is the deviation value of the melting point measurement caused by the temperature reflection lag, wherein the temperature rise rate is 25 ℃/min. For the same slag sample, along with the increase of the temperature rise rate, the measured value of the melting point is increased, and the measured result is higher due to partial melting. Therefore, the influence of temperature response delay, melting, 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 temperature response hysteresis is subtracted from the measured melting point, the theoretical melting point of the nonvolatile slag is obtained without changing with the change in the rate of temperature rise.
Evaluation of volatilization effect: extrapolation of curve 3 in fig. 2 yields point D, which is a measured melting point value when the temperature rise rate of the volatile slag tends to infinity, and this point reflects the measured melting point value obtained after the volatile slag has fully volatilized the volatile components, and the slag composition has changed significantly to zero, while the other points of curve 3 reflect the results of the combined actions of slag volatilization, temperature reflection lag, slag partial melting, and the like. Curve 2 is translated together with line 1 so that it coincides with point D at a point where the temperature tends towards zero, giving the result shown in figure 3. At this time, the shaded part between the translated curve 2 and the straight line 3 can show the influence of the temperature reflection lag and the partial melting of the volatile slag, the slag is prepared by considering the similar substances, the granularity, the compaction degree and the like are the same, and the lag phase in the determination process is basically consistent. The distance between curve 3 and curve 2 reflects the effect of volatilization on the measurement results, i.e., curve 2 is considered as the effect of "hysteresis + melting", curve 1 is considered as the effect of "volatilization", and the difference is the effect of "volatilization". Similarly, taking a temperature rise rate of 25 ℃/min as an example, the temperature difference corresponding to the line segment AB is the change of the melting point measurement value caused by temperature reflection lag and melting separation at a temperature rise rate of 25 ℃/min, and the temperature difference corresponding to the line segment AC is the change of the melting point measurement value caused by volatilization at a temperature rise rate of 25 ℃/min.
Measurement and calculation of theoretical melting point: since the value of the measured melting point value decreased by the decrease of the zero volatilization due to the decrease of the volatilization, that is, the decrease of the residence time at a high temperature due to the increase of the temperature rising rate, is the corresponding value of the line segment AC, the measured melting point value which can effectively suppress the volatilization of the slag should be compensated for by a certain amount at the corresponding point on the curve 3, and the corresponding point is shifted down to the result of the influence of the volatilization, that is, the result shown in the curve 4. That is, the slower the rate of temperature rise, the more volatile and the more compensatory. The temperature rise rate is about 30 ℃/min, the distance between the curve 2 and the curve 3 is basically unchanged, namely the influence of volatilization at the point is basically zero, and compensation is not needed at the moment. The lower the temperature rise rate, the more compensation. For this reason, the influence lines of the temperature response lag and the like in fig. 3 are shifted down to be aligned with the point E in fig. 4 (that is, this point is not compensated). Taking the temperature rise rate of 5 ℃/min as an example, if the volatilization can be effectively inhibited, the apparent measured value of the melting point is the corresponding value of an H point, but the melting point is increased due to the volatilization of volatile components, the melting point value measured by adopting the conventional semispherical point steelmaking slag melting point measuring method is a G point, the two have obvious deviation, and the line segment GH is the deviation, namely the compensation value to be given. Further, if the influence of temperature reaction lag or the like is eliminated, the melting point value should be the point corresponding to the straight line of the graph, i.e., the temperature corresponding to the point F, and this temperature should be the theoretical melting point of the corresponding slag (original composition), so that volatilization is suppressed and there is no reaction temperature lag. The melting point value is not changed along with the change of the temperature rising rate and the volatilization of the components.
(5) Evaluation of volatilization amount: and weighing the slag sample before and after the melting point is measured, estimating the content change of volatile components in the slag, and evaluating the influence of the volatilization of the slag containing the volatile components 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 volatilization of the slag on the melting point of the slag. In order to ensure accurate weighing, a precision balance with more than one ten-thousandth precision is adopted.
The following are specific application examples:
example 1
Evaluation of influence of volatilization in fluorine slag melting point measurement in electroslag remelting and result correction
Selecting slag and conventional melting point measurement
The slag composition of the medium fluorine slag for electroslag remelting is shown in table 1. All are mixed slag prepared by adopting chemical pure reagents.
TABLE 1 slag composition (wt/%) of medium fluorine slag for electroslag remelting
| Slag of furnace | Al2O3 | MgO | SiO2 | CaF2 | CaO |
| Medium fluorine slag | 29.33 | 2.57 | 9.15 | 30.12 | 28.83 |
| Fluorine-free slag | 18 | - | 42 | - | 40 |
And (3) measuring by using a hemisphere point, wherein the heating rate is 10 ℃/min, the hemisphere point of the fluorine-free slag obtained by measurement is 1351 ℃, and the corresponding melting point of the fluorine-free slag is 1432 ℃.
Mode of application
According to the method, the temperature of the hemispherical points of the two types of slag is measured by respectively adopting 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and 30 ℃/min, a change curve of a melting point along with the heating rate is drawn, and comprehensive influence values of 'temperature + slagging reaction + partial melting' and the like of the fluorine-free slag and corresponding influence values of 'temperature + slagging reaction + partial melting' and 'volatilization influence' of the fluorine slag are respectively obtained through coupling and extrapolation. And further extrapolating to obtain the melting point theoretical values of the medium-fluorine slag and the non-fluorine slag.
Application results
According to the method, when the comprehensive influence values of 'temperature + slagging reaction + melting separation' and the like are gradually increased to 30 ℃/min from 5 ℃/min along with the temperature rising 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 medium slag is gradually reduced to 1288 ℃ from 1380 ℃, and the influence of volatilization can reach 212 ℃ to the maximum extent. The melting point theoretical value of the fluorine slag obtained by further correction is 1225 ℃, and is basically close to 1240 ℃ of the measured value of the premelting slag with the same chemical composition (the volatilization of the premelting slag is far less than that of the mixed slag), thereby proving the credibility of the premelting slag.
Example 2
Evaluation of volatilization influence in melting point measurement of high-fluorine slag for electroslag remelting and result correction
Selecting slag and conventional melting point measurement
The high-fluorine slag for electroslag remelting has the slag composition shown in table 2, and is mixed slag prepared from chemical pure reagents.
TABLE 2 slag composition (wt/%) of melting point of high fluorine slag for electroslag remelting
| Slag of furnace | Al2O3 | SiO2 | CaF2 | CaO |
| High fluorine slag | 28.89 | 2.99 | 68.12 | - |
| Fluorine-free slag | 18 | 42 | - | 40 |
The hemisphere point is adopted for measurement, the heating rate is 10 ℃/min, the measured hemisphere point of the high fluorine slag is 1351 ℃, and the corresponding melting point of the fluorine-free slag is 1432 ℃.
Mode of application
According to the method, 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and 30 ℃/min are respectively adopted to measure the hemispherical point temperatures of the two types of slag, a change curve of a melting point along with the heating rate is drawn, and comprehensive influence values of 'temperature + slagging reaction + partial melting' and the like of the fluorine-free slag and corresponding respective influence values of 'temperature + slagging reaction + partial melting' and 'volatilization influence' of the fluorine slag are respectively obtained through coupling and extrapolation. And further extrapolating to obtain the melting point theoretical values of the medium-fluorine slag and the non-fluorine slag.
Application results
According to the method, when the comprehensive influence values of 'temperature + slagging reaction + melting separation' and the like are gradually increased to 30 ℃/min from 5 ℃/min along with the temperature rising 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 medium slag is gradually reduced to 1270 ℃ from 1351 ℃, and the influence of volatilization can reach 81 ℃ at most. Further correction is carried out to obtain the melting point theoretical value of the high-fluorine slag to be 1201 ℃.
Example 3
Evaluation of influence of volatilization in melting point measurement of steelmaking fluorine-containing covering slag and result correction
Selecting slag and conventional melting point measurement
One of the two continuous casting mold fluxes with the same chemical composition is mixed slag prepared by adopting a chemical pure reagent, and the other is pre-melted slag (after carbon is removed). The slag composition is shown in table 3 below,
TABLE 3 slag composition (wt/%) of fluorine-containing mold flux for steelmaking
And (3) measuring by adopting a hemisphere point, wherein the heating rate is 10 ℃/min, the temperature of the hemisphere point of the fluorine-containing covering slag mixed slag obtained by measurement is 1125 ℃, and the temperature of the corresponding hemisphere point of the pre-melted slag is 1032 ℃. The melting point of the fluorine-free mold flux is 1170 ℃.
Mode of application
According to the method, the temperature of the hemispherical points of the three types of furnace slag is measured by respectively adopting 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and 30 ℃/min, a change curve of a melting point along with the heating rate is drawn, and comprehensive influence values of 'temperature + slagging reaction + melting separation' and the like of the fluorine-free protective slag and respective influence values of 'temperature + slagging reaction + melting separation' and 'volatilization influence' of the corresponding fluorine-containing slag are respectively obtained through coupling and extrapolation. And further extrapolating to obtain a theoretical value of the melting point of the fluorine-containing covering slag mixed slag, and comparing with the result of measuring the melting point of the fluorine-containing slag pre-melted slag.
Application results
According to the method, when the comprehensive influence values of 'temperature + slagging reaction + melting separation' and the like are gradually increased to 30 ℃/min from 5 ℃/min along with the temperature rising rate, the apparent melting point value obtained by measuring the fluorine-free protective slag is gradually increased to 1211 ℃ from 1170 ℃; the apparent melting point value obtained by measuring the fluorine-containing mixed slag is gradually reduced to 1061 ℃ from 1125 ℃, so that the maximum volatilization influence can be inferred to be about 64 ℃. The melting point theoretical value of the fluorine-containing mold flux mixed slag obtained by further correction is 1020 ℃, and is basically close to 1032 ℃ of the measured value of the pre-melted slag with the same chemical composition (the volatilization of the pre-melted slag is far less than that of the mixed slag), thereby proving the credibility of the pre-melted slag.
Example 4 evaluation of influence of volatilization in measurement of melting Point of lead slag in vertical direct reduction and correction of result
Selecting slag and measuring conventional melting temperature
The lead slag composition in the direct lead reduction is shown in table 4. All are mixed slag prepared by adopting chemical pure reagents.
TABLE 4 slag composition (wt/%) of lead slag in vertical direct reduction
| Composition (I) | PbO | ZnO | CaO | FeO | SiO2 |
| Medium |
20 | 10 | 12.35 | 37.06 | 20.59 |
| Lead-free slag | - | 12.50 | 15.44 | 46.33 | 25.74 |
And (3) measuring by using a hemisphere point, wherein the heating rate is 10 ℃/min, the hemisphere melting temperature of the medium lead slag is 1226 ℃ and the corresponding melting temperature of the lead-free slag is 1292 ℃.
Mode of application
According to the method, the hemispherical point temperatures of two types of furnace slag are respectively measured by adopting 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min and 30 ℃/min, the change curves of the melting temperature along with the heating rates are drawn, the comprehensive influence values of 'temperature + slagging reaction + partial melting' and the like of the lead-free slag and the respective influence values of 'temperature + slagging reaction + partial melting' and 'volatilization influence' of the corresponding medium lead slag are respectively obtained through coupling and extrapolation, the influence evaluation on volatilization and other factors can be realized, and further, the theoretical melting temperature values of the medium lead slag and the lead-free slag are extrapolated.
Application results
According to the method, when the comprehensive influence values of 'temperature + slagging reaction + melting separation' and the like are gradually increased to 30 ℃/min from 5 ℃/min along with the temperature rise rate, the apparent melting temperature value measured on the lead-free slag is gradually increased to 1359 from 1286 ℃; the apparent melting temperature value measured by the medium lead slag is gradually reduced from 1263 ℃ to 1151 ℃, and the influence of volatilization can reach 208 ℃ to the maximum extent. The theoretical value of the melting temperature of the medium lead slag obtained by further correction is 1075 ℃, and is basically close to the measured value 1056 ℃ of the premelting slag with the same chemical composition (the volatilization of the premelting slag is far less than that of the mixed slag), thereby proving the credibility of the premelting slag.
Example 5
Evaluation of volatilization influence in measurement of melting point of high-lead slag in lead direct reduction and result correction
Selecting slag and measuring conventional melting temperature
The composition of the high lead slag in lead direct reduction is shown in table 5. All are mixed slag prepared by adopting chemical pure reagents.
TABLE 5 slag composition (wt/%) of high lead slag in vertical direct reduction
| Composition (I) | PbO | ZnO | CaO | FeO | SiO2 |
| Medium lead slag | 40 | 6 | 9.53 | 28.58 | 15.88 |
| Lead-free slag | - | 10.00 | 15.88 | 47.63 | 26.47 |
And (3) measuring by using a hemisphere point, wherein the heating rate is 10 ℃/min, the measured hemisphere melting temperature of the high-lead slag is 1206 ℃, and the corresponding melting temperature of the lead-free slag is 1296 ℃.
Mode of application
According to the method, the hemispherical point temperatures of two types of furnace slag are respectively measured by adopting 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min, 30 ℃/min and the like, a change curve of the melting temperature along with the heating rate is drawn, comprehensive influence values of 'temperature + slagging reaction + melting separation' and the like of the lead-free slag and respective influence values of 'temperature + slagging reaction + melting separation' and 'volatilization influence' of the corresponding medium lead slag are respectively obtained through coupling and extrapolation, the influence evaluation on volatilization and other factors can be realized, and further, the theoretical melting temperature values of the medium lead slag and the lead-free slag are extrapolated.
Application results
According to the method, when the comprehensive influence values of 'temperature + slagging reaction + melting separation' and the like are gradually increased to 30 ℃/min from 5 ℃/min along with the temperature rise rate, the apparent melting temperature value measured on the lead-free slag is gradually increased to 1364 ℃ from 1291 ℃; the apparent melting temperature value measured by the medium lead slag is gradually reduced from 1261 ℃ to 1130 ℃, and the influence of volatilization can reach 234 ℃ to the maximum extent. The theoretical value of the melting temperature of the lead slag obtained by further correction is 1053 ℃, and is basically close to the measured value of 1020 ℃ of the premelting slag with the same chemical composition (the volatilization of the premelting slag is far less than that of the mixed slag), thereby proving the credibility of the premelting slag.
Example 6
Evaluation of influence of volatilization in measurement of melting point of high lead slag in initial stage of vertical direct reduction and result correction
Selecting slag and measuring conventional melting temperature
The composition of the blast furnace slag at the initial stage of vertical direct reduction is shown in Table 6. All are mixed slag prepared by adopting chemical pure reagents.
TABLE 6 slag composition (wt/%) of initial lead-rich slag in vertical direct reduction
| Composition (I) | PbO | ZnO | CaO | FeO | SiO2 |
| Medium lead slag | 61.26 | 9.17 | 3.48 | 19.99 | 5.26 |
| Lead-free slag | - | 24.20 | 9.18 | 52.74 | 13.88 |
And (3) measuring by using a hemisphere point, wherein the heating rate is 10 ℃/min, the hemisphere melting temperature of the high-lead slag obtained by measurement is 1113 ℃, and the corresponding melting temperature of the lead-free slag is 1215 ℃.
Mode of application
According to the method, the hemispherical point temperatures of two types of furnace slag are respectively measured by adopting 5 heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min, 30 ℃/min and the like, a change curve of the melting temperature along with the heating rate is drawn, comprehensive influence values of 'temperature + slagging reaction + melting separation' and the like of the lead-free slag and respective influence values of 'temperature + slagging reaction + melting separation' and 'volatilization influence' of the corresponding medium lead slag are respectively obtained through coupling and extrapolation, the influence evaluation on volatilization and other factors can be realized, and further, the theoretical melting temperature values of the medium lead slag and the lead-free slag are extrapolated.
Application results
According to the method, when the obtained comprehensive influence values of 'temperature + slagging reaction + melting separation' and the like are gradually increased to 30 ℃/min from 5 ℃/min along with the temperature rising 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 measured by the high lead slag is gradually reduced from 1168 ℃ to 955 ℃, and the influence of volatilization can reach 359 ℃ to the maximum extent. The theoretical value of the 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 with the same chemical composition (the volatilization of the premelting slag is far less than that of the mixed slag), thereby proving the credibility of the premelting slag.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (9)
1. A method for evaluating the influence of volatilization of slag containing volatile components on a melting point is characterized by comprising the following steps:
measuring the melting point of the same slag containing the volatile components at different heating rates to obtain a corresponding relation curve of the melting point and the heating rate of the slag containing the volatile components;
measuring the melting point of the same slag without the volatile component at different heating rates to obtain a corresponding relation curve of the melting point of the slag without the volatile component and the heating rate;
extrapolating to obtain a measured value of the melting point of the non-volatile slag with the temperature rising rate tending to zero when the temperature rising rate is 0 according to a corresponding relation curve of the melting point of the non-volatile component slag and the temperature rising rate;
extrapolating to obtain the measured value of the melting point of the volatile slag with the temperature rising rate tending to zero when the temperature rising rate is 0 according to the corresponding relation curve of the melting point of the slag containing the volatile component and the temperature rising rate;
moving a corresponding relation curve of the melting point of the slag without the volatile component and the heating rate downwards to a state that a measured value of the melting point of the slag without the volatile component is coincident with a measured value of the melting point of the volatile slag, wherein the difference value of the two melting points of the slag corresponding to the same heating rate is an influence value of the volatilization of the slag on the melting point of the slag;
and subtracting the influence value of the slag volatilization on the slag melting point from the melting point of the corresponding relation curve of the melting point and the heating rate of the slag containing the volatile component to obtain the corresponding relation curve of the melting point and the heating rate which are not influenced by the volatilization, and then, when the heating rate is 0, obtaining the theoretical value of the melting point of the slag containing the volatile component.
2. The method of claim 1, wherein the influence of volatilization of the slag containing volatile components on the melting point is evaluated by hemispherical melting point measurement when determining the corresponding relationship between the melting point of the slag and the temperature increase rate.
3. The method of claim 1, wherein one of differential thermal analysis, ash melting point measurement and cone sample measurement is used to determine the relationship between the melting point of the slag and the temperature increase rate.
4. The method for evaluating the influence of volatilization of the slag containing the volatile components on the melting point according to claim 1, wherein the temperature rise rate is in a range of 5-30 ℃/min.
5. The method for evaluating the influence of volatilization of the slag containing the volatile components on the melting point according to claim 4, wherein the temperature rise rate is within the range of 5-30 ℃/min, and 4 or more temperature rise rate values are adopted for temperature rise.
6. The method of claim 1, wherein the temperature increase rate is at most 30 ℃/min or 35 ℃/min.
7. The method for evaluating the influence of the volatilization of the slag containing the volatile components on the melting point according to claim 1, wherein samples of the slag to be measured are weighed before and after all the melting points are measured, so that the content change of the volatile components in the slag is obtained, and the influence of the volatilization of the slag containing the volatile components 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 volatilization of the slag on the melting point of the slag.
8. The method for evaluating the influence of the volatilization of the slag containing the volatile components on the melting point according to claim 7, wherein a balance with a measurement accuracy of 0.0001g or more is used for weighing a sample of the slag to be measured.
9. The method of any one of claims 1 to 8, wherein the temperature increase rate is increased when the melting point of the volatile component-containing slag having high volatility is measured.
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