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
一种测定高温冶金熔渣流变特性的装置及方法,装置包括电加热炉、坩埚、流变仪和温度控制系统;电加热炉固定在升降装置上,坩埚固定在炉管内,流变仪的吊钩连接转子,转子位于坩埚内。方法为:(1)将渣样化渣破碎,置于坩埚中;(2)向炉管内通入保护气体并保持流通;通过电加热炉将渣样加热形成熔渣并保温;(3)控制炉管内的温度降温,在降温过程中测试熔渣的流变性质,采集分析数据;(4)根据流变仪测得的不同剪切速率下对应的剪切应力,建立熔渣流变学本构方程,确定熔渣的流变特性参数。本发明的装置及方法能快速准确地测试出高温熔渣的流变特性。
A device and method for measuring the rheological properties of pyrometallurgical slag, the device includes an electric heating furnace, a crucible, a rheometer and a temperature control system; the electric heating furnace is fixed on the lifting device, the crucible is fixed in the furnace tube, and the rheometer The hook is attached to the rotor, which is located inside the crucible. The method is: (1) break the slag sample into slag and place it in a crucible; (2) pass protective gas into the furnace tube and keep it in circulation; The temperature in the furnace tube is lowered, and the rheological properties of the slag are tested during the cooling process, and the analysis data is collected; (4) According to the corresponding shear stress at different shear rates measured by the rheometer, a slag rheological book is established Constructive equations to determine the rheological parameters of slag. The device and method of the invention can quickly and accurately test the rheological properties of high-temperature slag.
Description
技术领域 technical field
本发明属于冶金技术领域,特别涉及一种测定高温冶金熔渣流变特性的装置及方法。 The invention belongs to the technical field of metallurgy, in particular to a device and method for measuring the rheological properties of high-temperature metallurgical slag.
背景技术 Background technique
高温冶金熔渣主要由冶金原料中的氧化物或冶金过程中生成的氧化物组成的熔体;高温冶金熔渣在冶炼工艺上起重要作用;高温冶金熔渣主要是由氧化物构成,其成分与耐火材料液相十分相似,可以认为耐火材料液相有可能起到与熔渣相似的作用。实际上,在高温下一旦有一定数量的液相存在,耐火氧化物颗粒被液相所包裹,与熔融钢铁直接接触的是液相而不是耐火氧化物。高温冶金熔渣是一种高温溶液,其结构很复杂,至今仍未完全研究清楚。 Pyrometallurgical slag is mainly a melt composed of oxides in metallurgical raw materials or oxides generated during the metallurgical process; high-temperature metallurgical slag plays an important role in the smelting process; high-temperature metallurgical slag is mainly composed of oxides, and its composition It is very similar to the liquid phase of the refractory material, and it can be considered that the liquid phase of the refractory material may play a similar role to the slag. In fact, once a certain amount of liquid phase exists at high temperature, the refractory oxide particles are wrapped by the liquid phase, and the liquid phase is not the refractory oxide that is in direct contact with the molten steel. Pyrometallurgical slag is a kind of high-temperature solution, and its structure is very complex, which has not been fully studied until now.
火法冶金过程按冶炼方法和产品等的不同可产生各种冶金炉渣,而且炉渣性质的差异可以直接影响到冶金过程及各类冶金产品的质量;由于炉渣的组成、结构和质点间相互作用形式复杂,所以高温冶金熔渣的理论研究进展缓慢。 The pyrometallurgical process can produce various metallurgical slags according to different smelting methods and products, and the difference in the properties of the slag can directly affect the quality of the metallurgical process and various metallurgical products; Complex, so the theoretical research on pyrometallurgical slag progresses slowly.
一般认为熔渣在较高温度下是牛顿流体,但在熔渣中存在气、固相质点或产生硅酸盐的网状结构时会表现出非牛顿流体的特性,尤其我国矿产资源多金属共生的特点,使高温冶金熔渣的组元及结构更加复杂而远远偏离了牛顿流体,如我国钒钛磁铁矿高炉冶炼产生的含钛高炉渣。长期研究和工业实践证实,若含钛高炉渣中钛仅以TiO2或CaO·TiO2等形式存在,不会给高炉冶炼造成很大困难。但在高温和强还原条件下,熔渣中的部分TiO2被还原成高熔点的TiC、TiN及其固溶体Ti(C,N),这些钛化合物通常以高度分散的微小固体颗粒形态弥散于液态炉渣中,形成气-固-液三相复杂体系,从而引起炉渣急剧变稠、流动性变差、渣中带铁以及形成泡沫渣等一系列特殊问题,给钒钛磁铁矿高炉冶炼带来困难。目前关于含钛高炉渣的生成、演变规律开展了较多的理论研究,但对其流变特性及其转变规律等问题的认识仍显得模糊和不足,相关研究落后于工业化生产实践。另外,现有高温冶金熔渣理论体系基本都是建立在均相、牛顿流体基础之上,故有很大的局限性;而实际高温冶金熔渣多为非均相非牛顿熔体,因此亟待引入新的理论和研究思路,选择正确的研究和测试方法,系统开展这类熔体的流变特性及其转变规律研究。 It is generally believed that slag is a Newtonian fluid at higher temperatures, but it will show the characteristics of non-Newtonian fluid when there are gas and solid phase particles in the slag or a silicate network structure, especially the polymetallic symbiosis of mineral resources in my country. The characteristics of high-temperature metallurgical slag make the composition and structure of high-temperature metallurgical slag more complex and deviate far from Newtonian fluid, such as the titanium-containing blast furnace slag produced by blast furnace smelting of vanadium-titanium magnetite in my country. Long-term research and industrial practice have proved that if titanium in titanium-containing blast furnace slag exists only in the form of TiO 2 or CaO·TiO 2 , it will not cause great difficulties in blast furnace smelting. However, under high temperature and strong reducing conditions, part of the TiO2 in the slag is reduced to TiC, TiN and its solid solution Ti(C,N) with high melting point. These titanium compounds are usually dispersed in the liquid state in the form of highly dispersed tiny solid particles. In the slag, a gas-solid-liquid three-phase complex system is formed, which causes a series of special problems such as the rapid thickening of the slag, poor fluidity, iron in the slag, and the formation of foamy slag. difficulty. At present, many theoretical studies have been carried out on the formation and evolution of titanium-containing blast furnace slag, but the understanding of its rheological characteristics and transformation laws is still vague and insufficient, and the relevant research lags behind the industrial production practice. In addition, the existing theoretical system of pyrometallurgical slag is basically based on homogeneous and Newtonian fluids, so it has great limitations; however, most of the actual pyrometallurgical slags are heterogeneous and non-Newtonian melts, so it is urgent to Introduce new theories and research ideas, choose correct research and testing methods, and systematically carry out research on the rheological properties and transformation laws of this type of melt.
90年代初,Flemings首次将流变学的理论应用于液态金属半固态加工过程中出现的固液两相非牛顿熔体,很好地解释了液态金属的凝固过程,从而开拓了人们应用流变学原理解决非均相非牛顿熔体的诸多物理化学问题的新途径。采用流变学方法深入研究均相牛顿熔渣向非均相非牛顿熔渣的转变过程与规律,对全面认识高温冶金熔渣的流变特性十分有利,但遗憾的是,这方面的研究十分有限。 In the early 1990s, Flemings first applied the theory of rheology to the solid-liquid two-phase non-Newtonian melt that appeared in the semi-solid processing of liquid metal, which explained the solidification process of liquid metal well, thus opening up people's application of rheology. It is a new way to solve many physical and chemical problems of heterogeneous non-Newtonian melts. The use of rheological methods to study the transformation process and law of homogeneous Newtonian slag to heterogeneous non-Newtonian slag is very beneficial to a comprehensive understanding of the rheological properties of pyrometallurgical slag, but unfortunately, research in this area is very limited. limited.
目前,对于高温熔体的流变特性多采用拟牛顿流体测量方法,这是一种相对的测量方法,即将未知流体特性的熔体先按牛顿流体处理,高温旋转粘度计在选定某一固定转速时,可测得该转速下熔体的粘度η,在用旋转法测量粘度时,由于坩埚、测头的尺寸确定,所以旋转运动产生的剪切速率D只是转速的函数;根据不同的转速求出相应的剪切速率,再根据该转速下测得的粘度η,由公式τ = η D可求得剪切应力τ;根据不同D值时的τ值,作出流体的τ-D曲线,即流体的流变特性曲线,进而求出流体的本构方程;根据本构方程的形式和D的指数n(n是流动指数)大于1、等于1或小于1,进而判断流体属于牛顿流体还是非牛顿流体;但是,这种方法步骤繁琐,而且实验误差不好控制,计算出的结果准确度不高。 At present, the quasi-Newtonian fluid measurement method is mostly used for the rheological properties of high-temperature melts. This is a relative measurement method, that is, the melt with unknown fluid properties is treated as Newtonian fluid first, and the high-temperature rotational viscometer When the rotation speed is high, the viscosity η of the melt at this rotation speed can be measured. When the viscosity is measured by the rotation method, since the size of the crucible and the probe is determined, the shear rate D generated by the rotation motion is only a function of the rotation speed; according to different rotation speeds Find the corresponding shear rate, and then according to the viscosity η measured under the rotating speed, the shear stress τ can be obtained by the formula τ = η D ; according to the τ value during different D values, the τ - D curve of the fluid is made, That is, the rheological characteristic curve of the fluid, and then obtain the constitutive equation of the fluid; according to the form of the constitutive equation and the index n of D (n is the flow index) greater than 1, equal to 1 or less than 1, and then judge whether the fluid belongs to Newtonian fluid or Non-Newtonian fluid; however, this method has cumbersome steps, and the experimental error is not easy to control, and the accuracy of the calculated results is not high.
发明内容 Contents of the invention
针对现有高温冶金熔渣流变特性的测定技术存在的上述不足,本发明提供一种测定高温冶金熔渣流变特性的装置及方法,在降温过程中对渣样分别进行测试,根据不同剪切速率对应的剪切应力,建立本构方程,根据实际测量结果直接得到熔渣的本构方程,方便分析判断熔渣的流体类型。 Aiming at the above-mentioned deficiencies existing in the measurement technology of the rheological properties of the pyrometallurgical slag, the present invention provides a device and method for measuring the rheological properties of the pyrometallurgical slag. During the cooling process, the slag samples are tested separately. According to the shear stress corresponding to the shear rate, the constitutive equation is established, and the constitutive equation of the slag is directly obtained according to the actual measurement results, which is convenient for analysis and judgment of the fluid type of the slag.
本发明的测定高温冶金熔渣流变特性的装置包括电加热炉、坩埚、流变仪和温度控制系统;电加热炉固定在升降装置上,坩埚固定在电加热炉的炉管内部,流变仪的吊钩通过转杆与转子连接,转子位于坩埚内部;炉管底部设有气体通道,炉管内的热电偶与温度控制系统装配在一起,电加热炉内的发热体与温度控制系统装配在一起,流变仪与计算机装配在一起,温度控制系统与计算机连接。 The device for measuring the rheological properties of pyrometallurgical slag of the present invention includes an electric heating furnace, a crucible, a rheometer and a temperature control system; the electric heating furnace is fixed on the lifting device, the crucible is fixed inside the furnace tube of the electric heating The hook of the instrument is connected to the rotor through the rotating rod, and the rotor is located inside the crucible; there is a gas channel at the bottom of the furnace tube, the thermocouple in the furnace tube is assembled with the temperature control system, and the heating element in the electric heating furnace is assembled with the temperature control system. Together, the rheometer is assembled with a computer, and the temperature control system is connected with the computer.
上述的电加热炉的炉体内部设有保温材料,保温材料内部设有一个空腔,发热体下部位于空腔内。 The furnace body of the above-mentioned electric heating furnace is provided with insulation material inside, and a cavity is provided inside the insulation material, and the lower part of the heating element is located in the cavity.
上述的电加热炉的炉管顶部设有转杆通孔,转杆通孔与转杆之间有间隙;炉管底部设有坩埚座,坩埚位于炉管内的坩埚座上,且坩埚位于保温材料内部的空腔中。 The top of the furnace tube of the above-mentioned electric heating furnace is provided with a through hole of the rotating rod, and there is a gap between the through hole of the rotating rod and the rotating rod; the bottom of the furnace tube is provided with a crucible seat, and the crucible is located on the crucible seat in the furnace tube, and the crucible is located on the insulation material. in the internal cavity.
上述的热电偶插入炉管底部。 The aforementioned thermocouples are inserted into the bottom of the furnace tube.
上述的炉管底部的气体通道通过管道与气瓶连通。 The gas channel at the bottom of the above-mentioned furnace tube communicates with the gas bottle through a pipeline.
上述的升降装置固定在支撑架上,支撑架上还设有固定平台,流变仪固定在固定平台上。 The lifting device mentioned above is fixed on the supporting frame, and the supporting frame is also provided with a fixed platform on which the rheometer is fixed.
上述的转子材质为钼。 The material of the above-mentioned rotor is molybdenum.
上述的转杆材质为刚玉。 The above-mentioned rotating rod is made of corundum.
上述的坩埚材质为石墨且内壁设有内衬,内衬材质为钼。 The material of the above-mentioned crucible is graphite and the inner wall is provided with a lining, and the material of the lining is molybdenum.
本发明的测定高温冶金熔渣流变特性的方法是采用上述装置,按以下步骤进行: The method for measuring the rheological properties of pyrometallurgical slag of the present invention is to adopt the above-mentioned device, and carry out according to the following steps:
1、将渣样化渣破碎,置于坩埚中; 1. Break the slag-like slag and place it in the crucible;
2、向炉管内通入保护气体并保持流通;通过电加热炉将渣样加热至1500±10℃形成熔渣,保温至少1h; 2. Introduce protective gas into the furnace tube and keep it in circulation; heat the slag sample to 1500±10°C through an electric heating furnace to form molten slag, and keep it warm for at least 1 hour;
3、通过温度控制系统控制炉管内的温度降温,在降温过程中,通过流变仪测试熔渣的流变性质,并通过计算机采集分析数据,直至数据超过流变仪量程; 3. The temperature in the furnace tube is controlled by the temperature control system to cool down. During the cooling process, the rheological properties of the slag are tested by the rheometer, and the data is collected and analyzed by the computer until the data exceeds the range of the rheometer;
4、根据流变仪测得的不同剪切速率下对应的剪切应力,建立熔渣流变学本构方程,确定熔渣的流变特性参数。 4. According to the corresponding shear stress at different shear rates measured by the rheometer, establish the rheological constitutive equation of the slag, and determine the rheological characteristic parameters of the slag.
上述的步骤3中,流变仪测试的温度范围在1350~1500℃,每隔25±1℃进行一次测量。 In the above step 3, the temperature range of the rheometer test is 1350~1500°C, and a measurement is performed every 25±1°C.
上述方法中,通过流变仪测试渣样的流变性质时,转子的剪切速率为2.5~43.4s-1。 In the above method, when the rheological properties of the slag sample are tested by a rheometer, the shear rate of the rotor is 2.5~43.4s -1 .
上述的本构方程采用Herschel-Bulkley模型:τ=τy+kDn;其中,τ为剪切应力,单位为Pa;τy为屈服应力,单位为Pa;k为粘性因子;D为剪切速率,单位为s-1;n为流动指数。 The above constitutive equation adopts the Herschel-Bulkley model: τ=τ y +kD n ; where τ is the shear stress in Pa; τ y is the yield stress in Pa; k is the viscosity factor; D is the shear Speed, the unit is s -1 ; n is the flow index.
上述的保护气体为氩气或氮气。 The above-mentioned protective gas is argon or nitrogen.
上述的流变仪为使用温度-100℃~300℃的低温流变仪。 The above-mentioned rheometer is a low-temperature rheometer with an operating temperature of -100°C to 300°C.
本发明的装置及方法能快速准确地测试出高温熔渣的流变特性,且测试精度高,成本低,操作简单,能更全面表征高温冶金熔渣的流变性能。 The device and method of the invention can quickly and accurately test the rheological properties of high-temperature slag, and has high testing accuracy, low cost, simple operation, and can more comprehensively characterize the rheological properties of high-temperature metallurgical slag.
附图说明 Description of drawings
图1为本发明的测定高温冶金熔渣流变特性的装置结构示意图;图中,1、计算机,2、温度控制系统,3、流变仪,4、吊钩,5、转杆,6、固定平台,7、炉管,8、炉体,9、发热体,10、保温材料,11、转子;12、坩埚,13、熔渣,14、热电偶,15、底盖,16、电动螺杆升降装置,17、支撑架,18、气瓶,19、坩埚座; Fig. 1 is the device structural representation of measuring pyrometallurgical slag rheological characteristic of the present invention; Among the figure, 1, computer, 2, temperature control system, 3, rheometer, 4, suspension hook, 5, rotating rod, 6, Fixed platform, 7, furnace tube, 8, furnace body, 9, heating element, 10, insulation material, 11, rotor; 12, crucible, 13, slag, 14, thermocouple, 15, bottom cover, 16, electric screw Lifting device, 17, support frame, 18, gas cylinder, 19, crucible seat;
图2为本发明实施例1中TiO2含量15%时的τ-D曲线图; Fig. 2 is TiO in the embodiment of the present invention 1 The τ-D curve figure when content 15%;
图3为本发明实施例1中TiO2含量20%时的τ-D曲线图; Fig. 3 is TiO in the embodiment of the present invention 1 The τ-D curve figure when content 20%;
图4为本发明实施例1中TiO2含量25%时的τ-D曲线图; Fig. 4 is TiO in the embodiment of the present invention 1 The τ-D curve figure when content 25%;
图5为本发明实施例1中TiO2含量30%时的τ-D曲线图; Fig. 5 is TiO in the embodiment of the present invention 1 The τ-D curve figure when content 30%;
图6为本发明实施例1中TiO2含量35%时的τ-D曲线图; Fig. 6 is TiO in the embodiment of the present invention 1 The τ-D curve figure when content 35%;
图7为本发明实施例2中TiC含量2%时的τ-D曲线图; Fig. 7 is the τ-D curve figure when TiC content 2% in the embodiment of the present invention 2;
图8为本发明实施例2中TiC含量4%时的τ-D曲线图; Fig. 8 is the τ-D graph when TiC content is 4% in the embodiment of the present invention 2;
图9为本发明实施例2中TiC含量6%时的τ-D曲线图; Fig. 9 is the τ-D curve diagram when TiC content is 6% in the embodiment of the present invention 2;
图10为本发明实施例2中TiC含量8%时的τ-D曲线图。 Fig. 10 is a τ-D curve diagram when the TiC content is 8% in Example 2 of the present invention.
具体实施方式 Detailed ways
本发明实施例中采用的流变仪型号为Brookfield DV-Ⅲ;配套使用的软件名为Brookfield application software。 The rheometer model that adopts in the embodiment of the present invention is Brookfield DV-Ⅲ; The software supporting use is called Brookfield application software.
本发明实施例中采用的温度控制系统为ADAM模块。 The temperature control system adopted in the embodiment of the present invention is an ADAM module.
本发明实施例中采用的渣样的成分按重量百分比含CaO 22~33%,SiO2 20~30%,MgO 8%,Al2O3 14%,TiO2 9~35%,TiC 2~8%。 The composition of the slag sample used in the examples of the present invention contains CaO 22~33%, SiO 2 20~30%, MgO 8%, Al 2 O 3 14%, TiO 2 9~35%, TiC 2~8 by weight percentage. %.
本发明实施例中坩埚内渣样的重量为140g。 The weight of the slag sample in the crucible in the embodiment of the present invention is 140g.
本发明实施例中的加热体为二硅化钼;电加热炉为二硅化钼电加热炉 The heating body in the embodiment of the present invention is molybdenum disilicide; the electric heating furnace is molybdenum disilicide electric heating furnace
本发明实施例中的保温材料为市购氧化铝质耐火砖和氧化铝质空心球。 The insulation materials in the embodiment of the present invention are commercially available alumina refractory bricks and alumina hollow balls.
本发明实施例中应用Brookfield application software软件,对实验测量数据采用Herschel-Bulkley模型进行回归处理,并用蓖麻油(标准牛顿流体)对实验误差进行标定和处理;(对于回归方程中的屈服应力τy,若该值小于0,则不符合能量守恒原理,按0处理;若大于0,则需比较其忽略与否对粘性因子影响的误差;;选择17.5℃时蓖麻油(标准牛顿流体)标定实验中τy的最大容许偏差(7.67%),将该值作为判断是否忽略回归方程中τy的依据;即,回归方程中τy值小于和等于7.67%的都将忽略;同样,当回归方程中的流动指数n不为1时,则以17.5℃时蓖麻油的最大相对误差σ(10.6%)作为比较n是否为1的依据;相对误差计算公式为σ=|Dn-D1.00⁄D1.00|x100%,计算时D值取每次测量实验中的最大剪切速率值43.4s-1;如果回归方程的σ值小于蓖麻油实验最大相对误差10.6%时,则n值修正为1,此时本构方程按n=1给出)。 Application Brookfield application software software in the embodiment of the present invention, adopt Herschel-Bulkley model to carry out regression processing to experimental measurement data, and use castor oil (standard Newtonian fluid) to carry out calibration and process to experimental error; (for the yield stress τ y in the regression equation , if the value is less than 0, it does not conform to the principle of energy conservation, and it is treated as 0; if it is greater than 0, it is necessary to compare the error of its influence on the viscosity factor whether it is ignored or not; ; choose castor oil (standard Newtonian fluid) calibration experiment at 17.5°C The maximum allowable deviation (7.67%) of τ y in the regression equation, this value is used as the basis for judging whether to ignore τ y in the regression equation; that is, the value of τ y in the regression equation is less than or equal to 7.67% will be ignored; similarly, when the regression equation When the fluidity index n in is not 1, the maximum relative error σ (10.6%) of castor oil at 17.5°C is used as the basis for comparing whether n is 1; the relative error calculation formula is σ=|D n -D 1.00 ⁄D 1.00 |x100%, the D value is taken as the maximum shear rate value 43.4s -1 in each measurement experiment during calculation; if the σ value of the regression equation is less than the maximum relative error of the castor oil experiment of 10.6%, then the n value is corrected to 1, At this time, the constitutive equation is given by n=1).
实施例1 Example 1
测定高温冶金熔渣流变特性的装置结构如图1所示,包括电加热炉、坩埚12、流变仪3、温度控制系统2和计算机1; The device structure for measuring the rheological properties of pyrometallurgical slag is shown in Figure 1, including an electric heating furnace, a crucible 12, a rheometer 3, a temperature control system 2 and a computer 1;
电加热炉固定在电动螺杆升降装置16上,电加热炉包括炉体8及其内部的炉管7、保温材料10和发热体9,保温材料10内部设有一个空腔,发热体9下部位于空腔内; The electric heating furnace is fixed on the electric screw lifting device 16. The electric heating furnace includes a furnace body 8 and the furnace tube 7 inside it, an insulating material 10 and a heating element 9. A cavity is arranged inside the insulating material 10, and the lower part of the heating element 9 is located at inside the cavity;
坩埚12固定在炉管7内部,流变仪3的吊钩4连接转杆5,转杆5底部与转子11连接,转子11位于坩埚12内部; The crucible 12 is fixed inside the furnace tube 7, the hook 4 of the rheometer 3 is connected to the rotating rod 5, the bottom of the rotating rod 5 is connected to the rotor 11, and the rotor 11 is located inside the crucible 12;
炉管7底部的底盖15上设有气体通道,炉管7内的热电偶14与温度控制系统2装配在一起,电加热炉内的发热体9与温度控制系统2装配在一起,流变仪3与计算机1装配在一起,温度控制系统2与计算机1连接; The bottom cover 15 at the bottom of the furnace tube 7 is provided with a gas channel, the thermocouple 14 in the furnace tube 7 is assembled with the temperature control system 2, the heating element 9 in the electric heating furnace is assembled with the temperature control system 2, and the rheology The instrument 3 is assembled with the computer 1, and the temperature control system 2 is connected with the computer 1;
炉管7顶部设有转杆通孔,转杆通孔与转杆5之间有间隙;炉管7底部设有坩埚座19,坩埚12位于炉管7内的坩埚座19上,且坩埚12位于保温材料10内部的空腔中; The top of the furnace tube 7 is provided with a through hole of the rotating rod, and there is a gap between the through hole of the rotating rod and the rotating rod 5; Located in the cavity inside the thermal insulation material 10;
热电偶14通过底盖15插入炉管7底部; The thermocouple 14 is inserted into the bottom of the furnace tube 7 through the bottom cover 15;
气体通道通过管道与气瓶18连通; The gas passage communicates with the gas cylinder 18 through a pipeline;
电动螺杆升降装置16固定在支撑架17上,支撑架17上还设有固定平台6,流变仪3固定在固定平台6上; The electric screw lifting device 16 is fixed on the support frame 17, the support frame 17 is also provided with a fixed platform 6, and the rheometer 3 is fixed on the fixed platform 6;
转子材质为钼,形状为纺锤形,转杆材质为刚玉;坩埚材质为石墨且内壁设有内衬,内衬材质为钼; The material of the rotor is molybdenum, the shape is spindle-shaped, and the material of the rotating rod is corundum; the material of the crucible is graphite and the inner wall is lined with molybdenum;
采用上述装置,流变特性测试方法按以下步骤进行: Using the above-mentioned device, the rheological property test method is carried out according to the following steps:
1、将渣样化渣破碎,置于坩埚中; 1. Break the slag-like slag and place it in the crucible;
2、向炉管内通入保护气体并保持流通;保护气体为氩气或氮气;通过电加热炉将渣样加热至1500±10℃形成熔渣,保温1h; 2. Introduce protective gas into the furnace tube and keep it in circulation; the protective gas is argon or nitrogen; heat the slag sample to 1500±10°C through an electric heating furnace to form molten slag, and keep it warm for 1h;
3、通过温度控制系统控制炉管内的温度降温,在降温过程中,通过流变仪测试熔渣的流变性质,并通过计算机采集分析数据,直至数据超过流变仪量程; 3. The temperature in the furnace tube is controlled by the temperature control system to cool down. During the cooling process, the rheological properties of the slag are tested by the rheometer, and the data is collected and analyzed by the computer until the data exceeds the range of the rheometer;
4、根据流变仪测得的不同剪切速率下对应的剪切应力,建立熔渣流变学本构方程,确定熔渣的流变特性参数; 4. According to the corresponding shear stress at different shear rates measured by the rheometer, the rheological constitutive equation of the slag is established to determine the rheological characteristic parameters of the slag;
流变仪测试的温度范围在1350~1500℃,每隔25±1℃进行一次测量;通过流变仪测试渣样的流变性质时,转子的剪切速率为2.5~43.4s-1;本构方程采用Herschel-Bulkley模型:τ=τy+kDn;其中,τ为剪切应力,单位为Pa;τy为屈服应力,单位为Pa;k为粘性因子;D为剪切速率,单位为s-1;n为流动指数; The temperature range of the rheometer test is 1350~1500°C, and the measurement is carried out every 25±1°C; when the rheological properties of the slag sample are tested by the rheometer, the shear rate of the rotor is 2.5~43.4s -1 ; The Herschel-Bulkley model is adopted for the construction equation: τ=τ y +kD n ; where τ is the shear stress in Pa; τ y is the yield stress in Pa; k is the viscosity factor; D is the shear rate in Pa is s -1 ; n is the flow index;
采用的渣样的成分如表1所示; The composition of the slag sample used is shown in Table 1;
表1(wt%) Table 1 (wt%)
以No.1实验为例,渣样成分按重量百分比含CaO 33%,SiO2 30%,MgO 8%,Al2O3 14%,TiO2 15%;在温度T=1500℃时,按本构方程,假设τy≠0,本构方程为τ=-1.1950+2.8815D0.9253,假设τy=0,本构方程为τ=2.4134D0.9745,此时相对误差(σ/%)为9.01,小于标准蓖麻油实验的最大相对误差10.6,故转换后方程τ=2.4134D1.00,流体类型为牛顿流体,此时拟合方程相关系数R2=0.9998; Taking No.1 experiment as an example, the composition of the slag sample contains 33% CaO, 30% SiO 2 , 8% MgO, 14% Al 2 O 3 , and 15% TiO 2 by weight percentage; Assuming τ y ≠ 0, the constitutive equation is τ=-1.1950+2.8815D 0.9253 , assuming τ y =0, the constitutive equation is τ=2.4134D 0.9745 , at this time the relative error (σ/%) is 9.01, The maximum relative error of the standard castor oil experiment is 10.6, so the converted equation τ=2.4134D 1.00 , the fluid type is Newtonian fluid, and the correlation coefficient of the fitting equation R 2 =0.9998;
由上述方法测得的不同温度下τ-D曲线分别如图2、3、4、5、6所示;由图可知:熔渣在降温过程中,当温度降至临界粘度温度时,熔渣粘度骤然增加,迅速固化,呈现出晶体渣的特征;随TiO2含量的增加,熔渣的高温粘度整体呈下降趋势;温度高于临界粘度温度(熔渣粘度陡升时对应的温度)时,熔渣表现为牛顿流体;温度低于临界粘度温度时,熔渣出现剪切稀化现象,熔渣表现为非牛顿假塑性流体。 The τ-D curves at different temperatures measured by the above method are shown in Figures 2, 3, 4, 5, and 6 respectively; it can be seen from the figures that: during the cooling process of the slag, when the temperature drops to the critical viscosity temperature, the slag The viscosity suddenly increases and solidifies rapidly, showing the characteristics of crystalline slag; with the increase of TiO 2 content, the high-temperature viscosity of the slag shows a downward trend as a whole; The slag behaves as a Newtonian fluid; when the temperature is lower than the critical viscosity temperature, the slag appears shear thinning phenomenon, and the slag behaves as a non-Newtonian pseudoplastic fluid.
实施例2 Example 2
测定高温冶金熔渣流变特性的装置结构同实施例1; The structure of the device for measuring the rheological properties of pyrometallurgical slag is the same as in Example 1;
流变特性测试方法同实施例1; Rheological property testing method is the same as embodiment 1;
采用的渣样的成分如表2所示; The composition of the slag sample used is shown in Table 2;
表2(wt%) Table 2 (wt%)
以No.1实验为例,渣样成分按重量百分比含CaO 30.73%,SiO2 27.94%,MgO 8%,Al2O3 14%,TiC 2%,TiO2 17.33%;在温度T=1500℃时,按本构方程,假设τy≠0,本构方程为τ=-0.0727+1.5356D0.9929,假设τy=0,本构方程为τ=1.5205D0.9953,相对误差(σ/%)为1.73,小于标准蓖麻油实验的最大相对误差10.6,转换后方程τ=1.5205D1.00,流体类型为牛顿流体,此时拟合方程相关系数R2=0.9998; Taking No.1 experiment as an example, the composition of the slag sample contains 30.73% by weight of CaO, 27.94% of SiO 2 , 8% of MgO, 14% of Al 2 O 3 , 2% of TiC, and 17.33% of TiO 2 ; , according to the constitutive equation, assuming τ y ≠ 0, the constitutive equation is τ=-0.0727+1.5356D 0.9929 , assuming τ y =0, the constitutive equation is τ=1.5205D 0.9953 , and the relative error (σ/%) is 1.73, less than the maximum relative error of the standard castor oil experiment 10.6, the converted equation τ=1.5205D 1.00 , the fluid type is Newtonian fluid, and the correlation coefficient of the fitting equation R 2 =0.9998;
由上述方法测得的不同温度下τ-D曲线分别如图7、8、9、10所示;由图可知:随熔渣中TiC含量的增加,熔渣粘度整体呈增加趋势;当TiC=2%且温度高于熔渣临界粘度温度时,熔渣表现为牛顿流体;温度低于临界粘度温度时,熔渣表现为非牛顿假塑性流体,并出现剪切稀化现象;当TiC≥4%时,熔渣内部产生屈服应力,此时熔渣随温度变化表现为非牛顿宾汉姆流体或塑性假塑性流体;增加TiC含量,熔渣内屈服应力增大,剪切稀化现象越显著。 The τ-D curves at different temperatures measured by the above method are shown in Figures 7, 8, 9, and 10 respectively; it can be seen from the figure that with the increase of TiC content in the slag, the overall viscosity of the slag increases; when TiC= 2% and the temperature is higher than the critical viscosity temperature of the slag, the slag behaves as a Newtonian fluid; when the temperature is lower than the critical viscosity temperature, the slag behaves as a non-Newtonian pseudoplastic fluid, and shear thinning occurs; when TiC≥4 %, yield stress is generated inside the slag, and the slag behaves as non-Newtonian Bingham fluid or plastic pseudoplastic fluid with temperature change; increasing the TiC content, the yield stress in the slag increases, and the shear thinning phenomenon is more significant .
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