CN104316439A - Device and method for determining rheological properties of high-temperature metallurgy molten slag - Google Patents
Device and method for determining rheological properties of high-temperature metallurgy molten slag Download PDFInfo
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Abstract
The invention provides a device and a method for determining rheological properties of high-temperature metallurgy molten slag. The device comprises an electric heating furnace, a crucible, a rheometer and a temperature control system, wherein the electric heating furnace is fixed on a hoisting device and the crucible is fixed in a furnace tube; a lifting hook of the rheometer is connected with a rotor; and the rotor is located in the crucible. The method comprises the following steps: (1) slagging and crushing a slag sample and putting the slag sample into the crucible; (2) introducing protective gas into the furnace tube and keeping circulated; heating the slag sample by the electric heating furnace to form the molten slag, and keeping the heat; (3) controlling the temperature in the furnace tube to be reduced and testing the rheological properties of the molten slag in a cooling process; collecting analytical data; and (4) establishing a molten slag rheological constitutive equation according to corresponding shearing stress at different shearing speeds, which is measured by the rheometer, and determining rheological property parameters of the molten slag. According to the device and the method, the rheological properties of the high-temperature metallurgy molten slag can be rapidly and accurately tested.
Description
Technical field
The invention belongs to metallurgical technology field, particularly a kind of device and method measuring pyrometallurgy slag rheological characteristics.
Background technology
Pyrometallurgy slag is primarily of the melt of the oxide composition generated in the oxide in metallurgical raw material or metallurgical process; Pyrometallurgy slag plays an important role on smelting process; Pyrometallurgy slag is mainly made up of oxide, its composition and fire resistive material liquid phase quite similar, can think that fire resistive material liquid phase likely plays the effect similar to slag.In fact, at high temperature once there be the liquid phase of some to exist, refractory oxide particle wrap up by liquid phase, what directly contact with molten steel is liquid phase instead of refractory oxide.Pyrometallurgy slag is a kind of pyrosol, and its structure is very complicated, does not study clear so far yet completely.
Pyrometallurgical processes can produce various metallurgical slag by the difference of smelting process and product etc., and the difference of slag properties directly can have influence on the quality of metallurgical process and all kinds of metallurgic product; Due to the composition of slag, structure and particle interphase interaction complex forms, so the theoretical research progress of pyrometallurgy slag is slow.
It is generally acknowledged that slag is Newtonian fluid at relatively high temperatures, but the characteristic of non-Newtonian fluid can be shown when there is the reticulate texture of gas, solid phase particle or generation silicate in slag, especially the feature of Mineral Resources in China many metals symbiosis, make the constituent element of pyrometallurgy slag and structure more complicated and deviate from Newtonian fluid far away, as the titanium-containing blast furnace slag that China's vanadium titano-magnetite blast furnace process produces.Study for a long period of time and industrial practice confirmation, if titanium is only with TiO in titanium-containing blast furnace slag
2or CaOTiO
2exist etc. form, very large difficulty can not be caused to blast furnace process.But under high temperature and strong reducing condition, the part TiO in slag
2be reduced into dystectic TiC, TiN and solid solution Ti (C thereof, N), these titanium compounds usually with the minute solid particles form disperse of high degree of dispersion in liquid slag, form gas-solid-liquid three-phase complex system, thus cause slag sharply retrogradation, mobility is deteriorated, be with iron in slag and form a series of specific questions such as foamed slag, brings difficulty to vanadium titano-magnetite blast furnace process.The current generation about titanium-containing blast furnace slag, development law have been carried out more theoretical research, but have still been seemed fuzzy and not enough to the understanding of its problem such as rheological characteristics and change law thereof, and correlative study lags behind Industrialized Production Practice.In addition, existing pyrometallurgy slag theoretical system is substantially all be based upon on homogeneous phase, Newtonian fluid basis, therefore has significant limitation; And actual pyrometallurgy slag mostly is heterogeneous non-Newtonian melt, therefore urgently introduce new theory and Research Thinking, select correct research and method of testing, system carries out rheological characteristics and the change law research thereof of this kind of melt.
The beginning of the nineties, rheol theory is applied to the solid-liquid two-phase non-Newtonian melt occurred in liquid metal semi-solid processing process by Flemings first, explain the process of setting of liquid metal well, thus opened up people and apply the new way that rheology principle solves many Physico-Chemical Problems of heterogeneous non-Newtonian melt.Adopt rheological method further investigation homogeneous phase newton slag to the transition process of heterogeneous non newtonian slag and rule, very favourable to the rheological characteristics of full appreciation pyrometallurgy slag, but regrettably, the research of this respect is very limited.
At present, Newtonian fluid measuring method is intended in the many employings of rheological characteristics for high-temperature fusant, and this is a kind of relative measuring method, and the melt by unknown fluid behaviour first presses Newtonian fluid process, High Temperature Rotating viscosity meter, when selected a certain fixed rotating speed, can record the viscosity of melt under this rotating speed
η, when measuring viscosity with rotary process, because the size of crucible, gauge head is determined, so the shear rate that rotary motion produces
dthe just function of rotating speed; Corresponding shear rate is obtained according to different rotating speeds, then according to the viscosity recorded under this rotating speed
η, by formula
τ=η Dshear stress can be tried to achieve
τ; According to difference
dduring value
τvalue, makes fluid
τ-
dcurve, i.e. the rheological characteristics curve of fluid, and then obtain the constitutive equation of fluid; Flow index according to the form of constitutive equation and the index n(n of D) be greater than 1, equal 1 or be less than 1, and then judge that fluid belongs to Newtonian fluid or non-Newtonian fluid; But this method step is loaded down with trivial details, and the bad control of experimental error, the result precision calculated is not high.
Summary of the invention
For the determination techniques above shortcomings of existing pyrometallurgy slag rheological characteristics, the invention provides a kind of device and method measuring pyrometallurgy slag rheological characteristics, in temperature-fall period, slag specimen is tested respectively, the shear stress corresponding according to different shear rate, set up constitutive equation, directly obtain the constitutive equation of slag according to actual measured results, convenient analysis judges the fluid type of slag.
The device of mensuration pyrometallurgy slag rheological characteristics of the present invention comprises electric furnace, crucible, flow graph and temperature control system; Electric furnace is fixed on jacking gear, and the boiler tube that crucible is fixed on electric furnace is inner, and the suspension hook of flow graph is connected with rotor by bull stick, and rotor is positioned at crucible inside; Be provided with gas passage bottom boiler tube, the thermopair in boiler tube and temperature control system are assembled together, and the heater in electric furnace and temperature control system are assembled together, and flow graph is together with computer assemblies, and temperature control system is connected with computing machine.
The furnace interior of above-mentioned electric furnace is provided with insulation material, and insulation material inside is provided with a cavity, and heater bottom is positioned at cavity.
The boiler tube top of above-mentioned electric furnace is provided with bull stick through hole, has gap between bull stick through hole and bull stick; Be provided with crucible holder bottom boiler tube, crucible is positioned on the crucible holder of boiler tube, and crucible is arranged in the cavity of insulation material inside.
Above-mentioned thermopair inserts bottom boiler tube.
Gas passage bottom above-mentioned boiler tube is communicated with gas cylinder by pipeline.
Above-mentioned jacking gear is fixed on bracing frame, and bracing frame is also provided with stationary platform, and flow graph is fixing on the stationary platform.
Above-mentioned rotor material is molybdenum.
Above-mentioned bull stick material is corundum.
Above-mentioned crucible material is graphite and inwall is provided with liner, and liner material is molybdenum.
The method of mensuration pyrometallurgy slag rheological characteristics of the present invention adopts said apparatus, carries out according to the following steps:
1, slag specimen slag is broken, be placed in crucible;
2, in boiler tube, pass into blanket gas and keep circulation; By electric furnace, slag specimen is heated to 1500 ± 10 DEG C and forms slag, be incubated at least 1h;
3, control the greenhouse cooling in boiler tube by temperature control system, in temperature-fall period, by the rheological properties of rheometer test slag, and analyze data by computer acquisition, until data exceed flow graph range;
4, shear stress corresponding under the different shear rate recorded according to flow graph, sets up slag rheology constitutive equation, determines the rheological characteristics parameter of slag.
In above-mentioned step 3, the temperature range of rheometer test, at 1350 ~ 1500 DEG C, carries out one-shot measurement every 25 ± 1 DEG C.
In said method, during rheological properties by rheometer test slag specimen, the shear rate of rotor is 2.5 ~ 43.4s
-1.
Above-mentioned constitutive equation adopts Herschel-Bulkley model: τ=τ
y+ kD
n; Wherein, τ is shear stress, and unit is Pa; τ
yfor yield stress, unit is Pa; K is Viscosity Factor; D is shear rate, and unit is s
-1; N is flow index.
Above-mentioned blanket gas is argon gas or nitrogen.
Above-mentioned flow graph is the low temperature flow graph of serviceability temperature-100 DEG C ~ 300 DEG C.
Device and method of the present invention can test out the rheological characteristics of high-temperature slag rapidly and accurately, and measuring accuracy is high, and cost is low, simple to operate, can characterize the rheological property of pyrometallurgy slag more comprehensively.
Accompanying drawing explanation
Fig. 1 is the apparatus structure schematic diagram of mensuration pyrometallurgy slag rheological characteristics of the present invention; In figure, 1, computing machine, 2, temperature control system, 3, flow graph, 4, suspension hook, 5, bull stick, 6, stationary platform, 7, boiler tube, 8, body of heater, 9, heater, 10, insulation material, 11, rotor; 12, crucible, 13, slag, 14, thermopair, 15, bottom, 16, electric screw jacking gear, 17, bracing frame, 18, gas cylinder, 19, crucible holder;
Fig. 2 is TiO in the embodiment of the present invention 1
2τ-D curve map during content 15%;
Fig. 3 is TiO in the embodiment of the present invention 1
2τ-D curve map during content 20%;
Fig. 4 is TiO in the embodiment of the present invention 1
2τ-D curve map during content 25%;
Fig. 5 is TiO in the embodiment of the present invention 1
2τ-D curve map during content 30%;
Fig. 6 is TiO in the embodiment of the present invention 1
2τ-D curve map during content 35%;
τ-D curve map when Fig. 7 is TiC content 2% in the embodiment of the present invention 2;
τ-D curve map when Fig. 8 is TiC content 4% in the embodiment of the present invention 2;
τ-D curve map when Fig. 9 is TiC content 6% in the embodiment of the present invention 2;
τ-D curve map when Figure 10 is TiC content 8% in the embodiment of the present invention 2.
Embodiment
The flow graph model adopted in the embodiment of the present invention is Brookfield DV-III; Matching used software is called Brookfield application software.
The temperature control system adopted in the embodiment of the present invention is ADAM module.
The composition of the slag specimen adopted in the embodiment of the present invention is by weight percentage containing CaO 22 ~ 33%, SiO
220 ~ 30%, MgO 8%, Al
2o
314%, TiO
29 ~ 35%, TiC 2 ~ 8%.
In the embodiment of the present invention, in crucible, the weight of slag specimen is 140g.
Calandria in the embodiment of the present invention is molybdenum disilicide; Electric furnace is molybdenum disilicide electric furnace
Insulation material in the embodiment of the present invention is commercial aluminum oxide refractory brick and aluminum oxide hollow ball.
Apply Brookfield application software software in the embodiment of the present invention, adopt Herschel-Bulkley model to carry out recurrences to measured data of experiment and process, and with castor oil (standard Newtonian fluid) experimental error demarcated and process; (for the yield stress τ in regression equation
yif this value is less than 0, then do not meet conservation of energy principle, by 0 process; If be greater than 0, then need to compare it and whether ignore the error that Viscosity Factor is affected; ; τ in castor oil (standard Newtonian fluid) calibration experiment when selecting 17.5 DEG C
ymaximum tolerance deviation (7.67%), using this value as judging whether to ignore τ in regression equation
yfoundation; That is, τ in regression equation
yvalue is less than and equals 7.67% all will ignore; Equally, when the flow index n in regression equation is not 1, then using the maximum relative error σ (10.6%) of castor oil when 17.5 DEG C as comparing the foundation whether n is 1; Relative error computing formula be σ=| D
n-D
1.00d
1.00| x100%, during calculating, D value gets the maximum shear rate value 43.4s in each experiments of measuring
-1; If when the σ value of regression equation is less than castor oil experiment maximum relative error 10.6%, then n value is modified to 1, and now constitutive equation provides by n=1).
Embodiment 1
The apparatus structure measuring pyrometallurgy slag rheological characteristics as shown in Figure 1, comprises electric furnace, crucible 12, flow graph 3, temperature control system 2 and computing machine 1;
Electric furnace is fixed on electric screw jacking gear 16, and electric furnace comprises the boiler tube 7 of body of heater 8 and inside thereof, insulation material 10 and heater 9, and insulation material 10 inside is provided with a cavity, and heater 9 bottom is positioned at cavity;
It is inner that crucible 12 is fixed on boiler tube 7, and the suspension hook 4 of flow graph 3 connects bull stick 5, is connected bottom bull stick 5 with rotor 11, and it is inner that rotor 11 is positioned at crucible 12;
Bottom 15 bottom boiler tube 7 is provided with gas passage, thermopair 14 in boiler tube 7 is assembled together with temperature control system 2, heater 9 in electric furnace is assembled together with temperature control system 2, and flow graph 3 and computing machine 1 are assembled together, and temperature control system 2 is connected with computing machine 1;
Boiler tube 7 top is provided with bull stick through hole, has gap between bull stick through hole and bull stick 5; Be provided with crucible holder 19 bottom boiler tube 7, crucible 12 is positioned on the crucible holder 19 of boiler tube 7, and crucible 12 is arranged in the cavity of insulation material 10 inside;
Thermopair 14 inserts bottom boiler tube 7 by bottom 15;
Gas passage is communicated with gas cylinder 18 by pipeline;
Electric screw jacking gear 16 is fixed on bracing frame 17, and bracing frame 17 is also provided with stationary platform 6, and flow graph 3 is fixed in stationary platform 6;
Rotor material is molybdenum, and shape is spindle, and bull stick material is corundum; Crucible material is graphite and inwall is provided with liner, and liner material is molybdenum;
Adopt said apparatus, rheological characteristics method of testing is carried out according to the following steps:
1, slag specimen slag is broken, be placed in crucible;
2, in boiler tube, pass into blanket gas and keep circulation; Blanket gas is argon gas or nitrogen; By electric furnace, slag specimen is heated to 1500 ± 10 DEG C and forms slag, insulation 1h;
3, control the greenhouse cooling in boiler tube by temperature control system, in temperature-fall period, by the rheological properties of rheometer test slag, and analyze data by computer acquisition, until data exceed flow graph range;
4, shear stress corresponding under the different shear rate recorded according to flow graph, sets up slag rheology constitutive equation, determines the rheological characteristics parameter of slag;
The temperature range of rheometer test, at 1350 ~ 1500 DEG C, carries out one-shot measurement every 25 ± 1 DEG C; During rheological properties by rheometer test slag specimen, the shear rate of rotor is 2.5 ~ 43.4s
-1; Constitutive equation adopts Herschel-Bulkley model: τ=τ
y+ kD
n; Wherein, τ is shear stress, and unit is Pa; τ
yfor yield stress, unit is Pa; K is Viscosity Factor; D is shear rate, and unit is s
-1; N is flow index;
The composition of the slag specimen adopted is as shown in table 1;
Table 1(wt%)
| No. | CaO | SiO 2 | MgO | Al 2O 3 | TiO 2 | ∑ | Basicity (CaO/SiO 2） |
| 1 | 33 | 30 | 8 | 14 | 15 | 100 | 1.10 |
| 2 | 30.38 | 27.62 | 8 | 14 | 20 | 100 | 1.10 |
| 3 | 27.76 | 25.24 | 8 | 14 | 25 | 100 | 1.10 |
| 4 | 25.14 | 22.86 | 8 | 14 | 30 | 100 | 1.10 |
| 5 | 22.52 | 20.48 | 8 | 14 | 35 | 100 | 1.10 |
For No.1 experiment, slag specimen composition is by weight percentage containing CaO 33%, SiO
230%, MgO 8%, Al
2o
314%, TiO
215%; When temperature T=1500 DEG C, by constitutive equation, suppose τ
y≠ 0, constitutive equation is τ=-1.1950+2.8815D
0.9253, suppose τ
y=0, constitutive equation is τ=2.4134D
0.9745, now relative error (σ/%) is 9.01, is less than the maximum relative error 10.6 of standard castor oil experiment, therefore equation τ=2.4134D after conversion
1.00, fluid type is Newtonian fluid, now fit equation coefficient R
2=0.9998;
Under the different temperatures recorded by said method, τ-D curve is respectively as shown in Fig. 2,3,4,5,6; As seen from the figure: slag is in temperature-fall period, and when temperature is down to critical viscosity temperature, viscosity coefficient of dross increases suddenly, rapid solidification, presents the feature of crystal slag; With TiO
2the increase of content, the high temperature viscosity entirety of slag is on a declining curve; When temperature is higher than critical viscosity temperature (temperature corresponding when viscosity coefficient of dross skyrockets), slag shows as Newtonian fluid; When temperature is lower than critical viscosity temperature, there is shear thinning phenomenon in slag, and slag shows as non newtonian pseudoplastic fluid.
Embodiment 2
Measure the apparatus structure of pyrometallurgy slag rheological characteristics with embodiment 1;
Rheological characteristics method of testing is with embodiment 1;
The composition of the slag specimen adopted is as shown in table 2;
Table 2(wt%)
| No. | CaO | SiO 2 | MgO | Al 2O 3 | TiC | TiO 2 | ∑ | Basicity (CaO/SiO 2） |
| 1 | 30.73 | 27.94 | 8 | 14 | 2 | 17.33 | 100 | 1.10 |
| 2 | 31.08 | 28.25 | 8 | 14 | 4 | 14.67 | 100 | 1.10 |
| 3 | 31.43 | 28.57 | 8 | 14 | 6 | 12.00 | 100 | 1.10 |
| 4 | 31.78 | 28.89 | 8 | 14 | 8 | 9.33 | 100 | 1.10 |
For No.1 experiment, slag specimen composition is by weight percentage containing CaO 30.73%, SiO
227.94%, MgO 8%, Al
2o
314%, TiC 2%, TiO
217.33%; When temperature T=1500 DEG C, by constitutive equation, suppose τ
y≠ 0, constitutive equation is τ=-0.0727+1.5356D
0.9929, suppose τ
y=0, constitutive equation is τ=1.5205D
0.9953, relative error (σ/%) is 1.73, is less than the maximum relative error 10.6 of standard castor oil experiment, equation τ=1.5205D after conversion
1.00, fluid type is Newtonian fluid, now fit equation coefficient R
2=0.9998;
Under the different temperatures recorded by said method, τ-D curve is respectively as shown in Fig. 7,8,9,10; As seen from the figure: with the increase of TiC content in slag, viscosity coefficient of dross entirety is in increase trend; As TiC=2% and temperature higher than slag critical viscosity temperature time, slag shows as Newtonian fluid; When temperature is lower than critical viscosity temperature, slag shows as non newtonian pseudoplastic fluid, and occurs shear thinning phenomenon; When TiC >=4%, slag inside produces yield stress, and now slag varies with temperature and shows as non newtonian Bingham liquid or plasticity pseudoplastic fluid; Increase TiC content, in slag, yield stress increases, and shear thinning phenomenon is more remarkable.
Claims (9)
1. measure a device for pyrometallurgy slag rheological characteristics, it is characterized in that comprising electric furnace, crucible, flow graph and temperature control system; Electric furnace is fixed on jacking gear, and the boiler tube that crucible is fixed on electric furnace is inner, and the suspension hook of flow graph is connected with rotor by bull stick, and rotor is positioned at crucible inside; Be provided with gas passage bottom boiler tube, the thermopair in boiler tube and temperature control system are assembled together, and the heater in electric furnace and temperature control system are assembled together, and flow graph is together with computer assemblies, and temperature control system is connected with computing machine.
2. the device of mensuration pyrometallurgy slag rheological characteristics according to claim 1, is characterized in that the boiler tube top of described electric furnace is provided with bull stick through hole, has gap between bull stick through hole and bull stick; Be provided with crucible holder bottom boiler tube, crucible is positioned on the crucible holder of boiler tube, and crucible is arranged in the cavity of insulation material inside.
3. the device of mensuration pyrometallurgy slag rheological characteristics according to claim 1, is characterized in that described jacking gear is fixed on bracing frame, bracing frame is also provided with stationary platform, and flow graph is fixing on the stationary platform.
4. the device of mensuration pyrometallurgy slag rheological characteristics according to claim 1, is characterized in that described rotor material is molybdenum; Described bull stick material is corundum.
5. the device of mensuration pyrometallurgy slag rheological characteristics according to claim 1, it is characterized in that described crucible material is graphite and inwall is provided with liner, liner material is molybdenum.
6. measure a method for pyrometallurgy slag rheological characteristics, it is characterized in that adopting device according to claim 1, carry out according to the following steps:
(1) slag specimen slag is broken, be placed in crucible;
(2) in boiler tube, pass into blanket gas and keep circulation; By electric furnace, slag specimen is heated to 1500 ± 10 DEG C and forms slag, be incubated at least 1h;
(3) control the greenhouse cooling in boiler tube by temperature control system, in temperature-fall period, by the rheological properties of rheometer test slag, and analyze data by computer acquisition, until data exceed flow graph range;
(4) shear stress corresponding under the different shear rate recorded according to flow graph, sets up slag rheology constitutive equation, determines the rheological characteristics parameter of slag.
7. the method for mensuration pyrometallurgy slag rheological characteristics according to claim 6, is characterized in that, in step (3), the temperature range of rheometer test, at 1350 ~ 1500 DEG C, carries out one-shot measurement every 25 ± 1 DEG C.
8. the method for mensuration pyrometallurgy slag rheological characteristics according to claim 6, when it is characterized in that the rheological properties by rheometer test slag specimen, the shear rate of rotor is 2.5 ~ 43.4s
-1.
9. the method for mensuration pyrometallurgy slag rheological characteristics according to claim 6, is characterized in that described constitutive equation adopts Herschel-Bulkley model: τ=τ
y+ kD
n; Wherein, τ is shear stress, and unit is Pa; τ
yfor yield stress, unit is Pa; K is Viscosity Factor; D is shear rate, and unit is s
-1; N is flow index.
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