CN113960244A - Method for measuring content of montmorillonite in metallurgical pellets - Google Patents

Method for measuring content of montmorillonite in metallurgical pellets Download PDF

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CN113960244A
CN113960244A CN202111176897.XA CN202111176897A CN113960244A CN 113960244 A CN113960244 A CN 113960244A CN 202111176897 A CN202111176897 A CN 202111176897A CN 113960244 A CN113960244 A CN 113960244A
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montmorillonite
metallurgical
methylene blue
iron
content
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杨大兵
岳志玲
刘琦
胡明欣
王飞洋
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Wuhan University of Science and Technology WHUST
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • G01N31/162Determining the equivalent point by means of a discontinuity
    • G01N31/164Determining the equivalent point by means of a discontinuity by electrical or electrochemical means

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Abstract

本发明公开了一种测定冶金球团中蒙脱石含量的方法。步骤包括:(1)取冶金球团铁料中不同部位的铁料各10.0g;(2)分别加入100ml水;(3)在加热装置中加热至100℃并保温10min;(4)加热后的冶金球团铁料水溶液冷却至室温,使用磁性材料将溶液中的铁吸出;(5)使用滴定管逐滴加入质量分数0.2%的亚甲基蓝至步骤(4)所得溶液中,磁力搅拌机搅拌后测定电导,直至每单位量亚甲基蓝所导致电导增加量第三次明显增加,记录亚甲基蓝总添加量T甲。本方法依赖于数据支撑,便于判断滴定终点;需要的试剂及设备较少,成本相对较低;操作简单,可以快速有效测量。The invention discloses a method for determining the content of montmorillonite in metallurgical pellets. The steps include: (1) taking 10.0g of iron materials from different parts of the metallurgical pellet iron material; (2) adding 100ml of water respectively; (3) heating to 100° C. in a heating device and keeping the temperature for 10 minutes; (4) after heating The metallurgical pellet iron aqueous solution was cooled to room temperature, and the iron in the solution was sucked out by using a magnetic material; (5) 0.2% methylene blue was added dropwise to the solution obtained in step (4) using a burette, and the conductance was measured after stirring with a magnetic stirrer. , until the increase in conductance per unit amount of methylene blue increases significantly for the third time, and record the total amount of methylene blue added. The method relies on data support, which is convenient for judging the end point of the titration; less reagents and equipment are required, and the cost is relatively low; the operation is simple, and the measurement can be performed quickly and effectively.

Description

Method for measuring content of montmorillonite in metallurgical pellets
Technical Field
The invention relates to the technical field of metallurgical pellet binders, in particular to a method for determining the content of montmorillonite in metallurgical pellets.
Background
Montmorillonite is used as the main component of the bentonite pellet binder, and has the main function of pelletizing the mineral powder, so that the mineral powder with low utilization rate can be better and fully utilized.
In order to ensure that the metallurgical pellets have the same properties, the binder in the pellets needs to be uniformly distributed.
The existing main methods for measuring the content of montmorillonite in metallurgical pellets comprise the following steps:
first, X-ray diffraction spectroscopy can be used;
second, after dispersing the sample with sodium phosphate, the sample was titrated with methylene blue and visually observed for the presence of a light green halo around the dark blue spot in the center of the titration.
However, the existing technology for measuring the content of montmorillonite in metallurgical pellets has the following great defects:
firstly, the operation is complex, and the rapid and effective measurement is difficult;
secondly, in the measurement, more reagents and equipment are needed, and the cost is relatively high;
thirdly, when the end point is measured, the color difference is difficult to distinguish; it is difficult to judge that the end point is reached.
Disclosure of Invention
The invention provides a method for measuring the montmorillonite content in metallurgical pellets aiming at the defects in the existing method for measuring the montmorillonite content in metallurgical pellets.
In order to achieve the purpose, the technical scheme adopted by the invention is a method for measuring the content of montmorillonite in metallurgical pellets, and the method comprises the following steps:
(1) taking 10.0g of iron materials at different parts in the metallurgical pellet iron material containing the montmorillonite adhesive;
(2) adding 100ml of water into the iron materials at different positions respectively;
(3) heating to 100 deg.C in a heating device and maintaining the temperature for 10 min;
(4) cooling the heated metallurgical pellet iron material water solution to room temperature, and sucking out iron in the solution by using a magnetic material;
(5) dropwise adding methylene blue with the mass fraction of 0.2% into the solution obtained in the step (4) by using a burette, measuring the conductance after stirring for a certain time by using a magnetic stirrer at a certain rotating speed until the third time of the conductance increase caused by each unit amount of the methylene blue is obviously increased, and recording the total addition amount Tjia of the methylene blue; the montmorillonite content of the metallurgical pellet iron material containing the montmorillonite adhesive is reflected by the finally measured total addition amount Tforma of methylene blue.
According to an embodiment of the invention, the magnetic material is a material of a ferromagnetic element comprising iron, cobalt, nickel.
According to the embodiment of the invention, the increase of the conductance in the step (5) refers to the increase of the conductance after and before the dropwise addition of every 0.5ml of methylene blue.
According to the embodiment of the invention, the unit amount of the methylene blue solution in the step (5) is 1ml, 0.5ml and 0.1ml according to the requirement of experimental precision.
According to the embodiment of the invention, in the step (5), the rotation speed of the magnetic stirrer is 500rpm, 800rpm, 1000rpm, 1200rpm and 1500rpm, and the stirring time is 1min, 2min and 5 min.
The working principle of the method for measuring the content of the montmorillonite in the metallurgical pellet is as follows:
(1) the main component bentonite of the montmorillonite binder is a clay mineral which takes montmorillonite as a main component, and the clay mineral has the capability of adsorbing methylene blue;
(2) the main components of the metallurgical pellets are iron powder and a binder; the iron powder has magnetic properties, while the binder does not. The magnetic substance can completely separate the iron powder from the binder; analyzing the concentration of iron ions in the water by using an iron ion analyzer, and if the concentration is lower than 1ppm, the iron powder and the binder can be considered to be completely separated;
(3) the temperature is raised, and the heat preservation is beneficial to separating the metallurgical pellets in pure water;
(4) the electrical conductance of the binder and methylene blue in water is greatly different.
The total addition amount Tforma of methylene blue measured at different parts can also reflect the uniform distribution degree of montmorillonite in the metallurgical pellets.
The montmorillonite adhesive refers to various bentonites.
When the magnetism of the metallurgical pellet iron material is stronger, a material with weaker magnetism can be used; when the magnetism of the iron material of the metallurgical pellet is weaker, a material with stronger magnetism can be used.
The magnetic strength standard of the metallurgical pellet iron material is that the iron grade is 60 percent, and the magnetic strength distinguishing standard of the magnetic material is 60 mT.
The method for determining the montmorillonite content in the metallurgical pellets has the following advantages:
(1) compared with the prior art which relies on the naked eye to observe chromatic aberration, the method relies on data support, and is convenient for judging the titration end point;
(2) the required reagent and equipment are less, and the cost is relatively low;
(3) the method is simple to operate and can be used for rapid and effective measurement.
Drawings
FIG. 1 shows the total amount Tformazan of methylene blue added at measurement point 1 of example.
FIG. 2 shows the total amount Tformazan of methylene blue added at measurement point 2 in example one.
FIG. 3 shows the average content of total addition Tformazan of methylene blue in the examples.
FIG. 4 shows X-ray diffraction spectroscopy measurements of one embodiment.
FIG. 5 shows the total amount of methylene blue added Tforma at measurement point 1 in example two.
FIG. 6 shows the total amount of methylene blue added Tforma at measurement point 2 in example two.
FIG. 7 shows the average content of total added amount Tformazan of dimethylene blue in example.
FIG. 8 shows the X-ray diffraction spectroscopy measurement values of the second example.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The first embodiment is as follows: a method for measuring the montmorillonite content in metallurgical pellets comprises the following steps:
(1) taking 10.0g of iron materials at different parts in the metallurgical pellet iron material containing the montmorillonite adhesive;
(2) adding the iron material obtained in the step (1) into a 250ml beaker, and adding 100ml of water;
(3) adding the product obtained in the step (2) into an phase heating device, heating to 100 ℃, and preserving heat for 10 min;
(4) cooling the metallurgical pellet iron material aqueous solution containing the montmorillonite adhesive obtained in the step (3) to room temperature, and then completely removing iron in the solution by using a magnetic material;
(5) and (3) dropwise adding methylene blue with the mass fraction of 0.2% into the solution obtained in the step (4) by using a burette, measuring the conductance after stirring the solution for 2min at the rotating speed of 1000rpm by using a magnetic stirrer until the third obvious increase of the conductance caused by each unit amount of the methylene blue is achieved, and recording the total addition amount Tjia of the methylene blue.
The measuring range of the conductivity meter is 0-2000 mu s/cm.
The montmorillonite content of the metallurgical pellet iron material containing the montmorillonite adhesive is reflected by the finally measured total addition amount Tforma of methylene blue.
May also be reflected in the content M formazan.
Figure 520901DEST_PATH_IMAGE001
The results of the examples are shown in FIGS. 1, 2 and 3, where T nails were 20 ml. + -. 2 at different sites and were considered to be uniformly distributed.
M nail =77.2% was calculated according to the formula.
The detection result of the X-ray diffraction spectrum method is 77.44 percent, which is similar to the measurement result of the invention.
1. Example two: a method for measuring the montmorillonite content in metallurgical pellets comprises the following steps:
(1) taking 10.0g of iron materials at different parts in the metallurgical pellet iron material containing the montmorillonite adhesive;
(2) adding the iron material obtained in the step 1 into a 250ml beaker, and adding 100ml of water;
(3) adding the product obtained in the step 2 into a phase heating device, heating to 100 ℃, and preserving heat for 10 min;
(4) cooling the metallurgical pellet iron material aqueous solution containing the montmorillonite adhesive obtained in the step 3 to room temperature, and then completely removing iron in the solution by using a magnetic material;
(5) and (3) dropwise adding methylene blue into the solution obtained in the step (4) by using a burette, measuring the electric conductivity after stirring for 5min at the rotating speed of 800rpm by a magnetic stirrer until the third obvious increase of the electric conductivity caused by every 1ml of methylene blue is achieved, and recording the total addition amount Tforma of the methylene blue.
The measuring range of the conductivity meter is 0-2000 mu s/cm.
The montmorillonite content of the metallurgical pellet iron material containing the montmorillonite adhesive is reflected by the finally measured total addition amount Tforma of methylene blue.
May also be reflected in the content M formazan.
Figure 551917DEST_PATH_IMAGE001
The results of the second example are shown in FIGS. 4, 5 and 6, and T nails at different sites were 18 ml. + -. 1, and the distribution was considered to be uniform.
M nail =69.70% was calculated according to the formula.
The detection result of the X-ray diffraction spectrum method is 69.24 percent, which is similar to the measurement result of the invention.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (5)

1.一种测定冶金球团中蒙脱石含量的方法,其特征步骤包括:1. a method for measuring montmorillonite content in metallurgical pellets, characterized in that the steps include: (1)取含有蒙脱石类粘性剂的冶金球团铁料中不同部位的铁料各10.0g;(1) Take 10.0g each of the iron materials in different parts of the metallurgical pelletized iron materials containing montmorillonite-type adhesives; (2)所述不同部位的铁料分别加入100ml水;(2) Add 100ml of water to the iron materials in different parts; (3)在加热装置中加热至100℃并保温10min;(3) Heating to 100℃ in a heating device and holding for 10min; (4)加热后的冶金球团铁料水溶液冷却至室温,使用磁性材料将溶液中的铁吸出;(4) The heated aqueous solution of metallurgical pellet iron material is cooled to room temperature, and the iron in the solution is sucked out by magnetic material; (5)使用滴定管逐滴加入质量分数0.2%的亚甲基蓝至步骤(4)所得溶液中,磁力搅拌机在一定转速下搅拌一定时长后测定电导,直至每单位量亚甲基蓝所导致电导增加量第三次明显增加,记录亚甲基蓝总添加量T甲;含有蒙脱石类粘性剂的冶金球团铁料中蒙脱石含量以最终所测定的亚甲基蓝总添加量T甲反映。(5) Use a burette to add 0.2% methylene blue dropwise to the solution obtained in step (4). The magnetic stirrer is stirred at a certain speed for a certain period of time and then the conductance is measured until the increase in conductance per unit amount of methylene blue is obvious for the third time. Increase, record the total addition amount of methylene blue T A; the content of montmorillonite in the metallurgical pellet iron containing smectite-type adhesive is reflected by the final measured total addition amount of methylene blue T A. 2.根据权利要求1所述的一种测定冶金球团中蒙脱石含量的方法,其特征在于所述磁性材料是含铁、钴、镍的铁磁性元素的材料。2 . The method for measuring the content of montmorillonite in metallurgical pellets according to claim 1 , wherein the magnetic material is a material containing ferromagnetic elements of iron, cobalt and nickel. 3 . 3.根据权利要求1所述的一种测定冶金球团中蒙脱石含量的方法,其特征在于所述步骤(5)电导增加量指每0.5ml亚甲基蓝滴加后与滴加前的电导增加量。3. A method for measuring the content of montmorillonite in metallurgical pellets according to claim 1, characterized in that the increase in conductance in the step (5) refers to the increase in conductance after the dropwise addition of every 0.5ml of methylene blue and before the dropwise addition. quantity. 4.根据权利要求1所述的一种测定冶金球团中蒙脱石含量的方法,其特征在于所述步骤(5)中单位量亚甲基蓝溶液根据实验精度需求,是1ml、0.5ml、0.1ml。4. The method for determining the content of montmorillonite in metallurgical pellets according to claim 1, wherein the unit amount of methylene blue solution in the step (5) is 1ml, 0.5ml, 0.1ml according to the experimental accuracy requirements . 5.根据权利要求1所述的一种测定冶金球团中蒙脱石含量的方法,其特征在于所述步骤(5)中磁力搅拌机转速是500rpm、800rpm、1000rpm、1200rpm、1500rpm,搅拌时间是1min、2min、5min。5. The method for measuring the content of montmorillonite in metallurgical pellets according to claim 1, wherein in the step (5), the rotating speed of the magnetic stirrer is 500rpm, 800rpm, 1000rpm, 1200rpm, 1500rpm, and the stirring time is 1min, 2min, 5min.
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CN114924028A (en) * 2022-04-29 2022-08-19 马鞍山钢铁股份有限公司 Method for determining binder distribution uniformity in iron ore concentrate
CN114924028B (en) * 2022-04-29 2024-04-26 马鞍山钢铁股份有限公司 Method for measuring binder distribution uniformity in iron ore concentrate

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