CN101329243A - Method for measuring iron ore crystal water content - Google Patents
Method for measuring iron ore crystal water content Download PDFInfo
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- CN101329243A CN101329243A CNA2008100554774A CN200810055477A CN101329243A CN 101329243 A CN101329243 A CN 101329243A CN A2008100554774 A CNA2008100554774 A CN A2008100554774A CN 200810055477 A CN200810055477 A CN 200810055477A CN 101329243 A CN101329243 A CN 101329243A
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Abstract
The invention provides a testing method used for measuring the water content of iron ore crystal water, which belongs to the field of detection technique and is used for solving the problems that the existing measuring equipments used for measuring the water content of the iron ore crystal water are complex and have high expense. The method of the invention consists of the steps as follows: preparing samples, samples entering the furnace, heating the samples, cooling the samples, and calculating the test results, etc. Based on the characteristic that the crystal water in limonite can be completely decomposed and the little carbonate in limonite is decomposed under the temperature of about 400 DEG C, the content of the iron ore crystal water is calculated according to the difference of the dried ore mass and the mass of the ore after the crystal water is overflowed; the method can utilize nationally specified coke reaction equipment generally used by current iron enterprises to carry out the measurement of crystal water of limonite, sufficiently plays the test functions of the existing equipments, and provides a feasible mean for self-measuring the iron ore crystal water for most iron enterprises without increasing other instruments. By the verification of a plurality of contrast tests, the method of the invention has the advantages of simpleness and feasibility, and exact test data.
Description
Technical field
The present invention relates to a kind of detection method, specifically, is to utilize the reactive equipment of coke, accurately measures the method for iron ore crystal water content, belongs to the detection technique field.
Background technology
Mainly show following two aspects as if containing of the influence of higher crystalline water in the iron ore to Iron and Steel Production: the one, for breeze, use the water of crystallization in the breeze not participate in the final component of sintering deposit in the SINTERING PRODUCTION, thereby can cause and join the ore deposit error, and after decomposition, cause the sintering feed cake to shrink by a relatively large margin, thereby influence the output and the quality of sintering deposit; On the other hand, understand explosion generation powder, influence smooth operation of furnace owing to the quick rising of temperature directly into the lump ore of stove.Therefore, produce in order to instruct better, the water of crystallization of the reply mineral that use is measured.At present, general limonite water of crystallization method is to be undertaken by the differential thermal analysis (DTA) instrument, that is: use heating arrangement that limonite is heated, measure according to the weight-loss curve of iron ore then, the shortcoming of this method is the experimental facilities complexity, expense is higher, and most of iron and steel enterprise is not equipped with this experimental facilities, and only carries out the scaling loss analysis.At present, most enterprises often need outer committee to carry out for the analysis of ore water of crystallization.
Continuous development along with Iron and Steel Production, increasing iron and steel enterprise has set up coke and the hot metallurgical performance of ore laboratory, the reactive experimental facilities of mensuration coke that utilizes these to popularize in iron and steel enterprise, seek a kind of method of measuring water of crystallization content in the iron ore, the production for iron and steel enterprise has significance undoubtedly.
Summary of the invention
The present invention is used to solve the defective of above-mentioned prior art and a kind of simple and easy to do, assay method that experimental data is used for iron ore crystal water content accurately is provided.
The alleged problem of the present invention is solved by following technical scheme:
A kind of assay method that is used for iron ore crystal water content, its special feature are that it carries out according to following steps:
A. produce sample: need measure ore and put into the baking box baking, 100～150 ℃ of baking temperatures, stoving time 60～180min takes out the back crushing screening, obtains
The sample of particle diameter;
B. sample is gone into stove: take by weighing 500g soil 0.1g sample, be designated as m
0, sample is inserted in the reaction tube, cover tight reaction tube loam cake, again reaction tube is put into heating furnace, the reaction tube charging temperature is controlled at below 200 ℃:
C. sample heating: sample heats in heating furnace, sets the Heating Furnace Control temperature to be
Set heating rate less than 30 ℃/min, with
Flow protect to the logical nitrogen of reaction tube, after temperature reaches controlling value, constant temperature 30～120min;
D. sample cooling: constant temperature takes out reaction tube after finishing in stove, continues to the logical nitrogen of reaction tube, stops logical nitrogen below the cooling terminal temperature to 100 ℃, opens the reaction tube loam cake, pours out sample, claims fixed its weight, is designated as m
1
E. test findings is calculated:
W in the formula
JWater of crystallization percentage composition for the iron ore of this part sample;
F. this sample repeat above-mentioned b, c, d, e step 3 time, 5 times or 7 times, get the mean value of each time test findings, be the water of crystallization percentage composition of the ore of measuring.
The above-mentioned assay method that is used for iron ore crystal water content, in the described sample heating steps when specimen temperature near or reach control during temperature, increase nitrogen flow to higher limit; In stove, take out reaction tube in the described sample cooling step, continue to lead to the flow control of nitrogen at 5L/min to reaction tube.
The above-mentioned assay method that is used for iron ore crystal water content, described reaction tube are coke or ore hot performance test reaction tube, and described heating furnace is the reactive heating furnace of coke.
The present invention is directed to existing iron ore crystal water content sensing equipment complexity, the expense problem of higher is improved, it can decompose about 400 ℃ of temperature fully based on the water of crystallization in the limonite and these characteristics of carbonate little disintegration wherein, the difference of overflowing the back ore quality with dried ore quality and water of crystallization is calculated the content of ore water of crystallization, the reactive equipment of the coke that the GB that this method can utilize present iron and steel enterprise generally to use is stipulated carries out the limonite ore water of crystallization, give full play to the test function of these existing equipments, under the prerequisite that does not increase Other Instruments equipment,, most of iron and steel enterprises provide the feasibility approach for measuring the ore water of crystallization voluntarily.Prove that this method has is simple and easy to do, experimental data advantage accurately through a large amount of contrast experiments.
Embodiment
Temperature-weight-loss curve that a large amount of by analysis differential thermal analysis (DTA) instruments mensuration of the present invention iron ore crystal water is made draws, water of crystallization in the limonite begins to decompose about 200 ℃, about 400 ℃ of temperature, decompose fully, water of crystallization overflows in the mode of steam, make and no longer contain water of crystallization in the ore, and carbonate little disintegration wherein.Dried ore (having removed mechanical water) quality m
0Overflow back ore quality m with water of crystallization
1Difference is exactly the quality of its contained water of crystallization, has designed water of crystallization method in the ore thus.Assay method device therefor of the present invention is the coke hot performance of GB regulation and ore low temperature reduction degradation, reduction degree testing equipment; the employed reaction tube of coke reactivity test wherein; the present invention is used as the closed container that holds the ore sample to it, and it can satisfy has protection gas to pass through the ore sample evenly, smoothly.Heating arrangement then uses the heating furnace and the temperature control system of coke or ore experiment.
Several specific embodiments below are provided:
Embodiment 1. gets sample ore A and puts into the baking box baking, 100 ℃ of baking temperatures, and stoving time 180min takes out the back crushing screening, obtains
The sample of particle diameter.
Take by weighing 500g soil 0.1g sample, be designated as m
0Sample is inserted in the reaction tube, cover tight reaction tube loam cake, reaction tube is put into the heating furnace flat-temperature zone again, the reaction tube charging temperature is controlled at below 200 ℃: setting the Heating Furnace Control temperature is 400 ℃, setting heating rate is 20 ℃/min, for preventing that the ferrous iron in the ore from reoxidizing, protect to the logical nitrogen of reaction tube with the flow of 2L/min, when temperature reaches 380 ℃, increase nitrogen flow to 10L/min, constant temperature 60min when temperature reaches 400 ℃; Constant temperature takes out reaction tube after finishing in stove, continue to the logical nitrogen of reaction tube, and flow control is cooled to terminal temperature and stops logical nitrogen below 100 ℃ at 5L/min, opens the reaction tube loam cake, pours out sample, claims fixed its weight, is designated as m
1
According to formula
Calculate the water of crystallization percentage composition of the iron ore of this part sample.
Continue to take by weighing this sample according to the method described above and according to above-mentioned test condition revision test, carry out three groups of samples mensuration altogether, result of calculation is as shown in the table:
| Experiment is inferior | 1 | 2 | 3 | Mean value |
| Water of crystallization content (%) | 7.3 | 7.4 | 7.2 | 7.3 |
Through aforementioned calculation, drawing sample ore A water of crystallization content is 7.3%.
Embodiment 2. gets sample ore B and puts into the baking box baking, 120 ℃ of baking temperatures, and stoving time 100min takes out the back crushing screening, obtains
The sample in footpath.
Take by weighing 500g soil 0.1g sample, be designated as m
0Sample is inserted in the reaction tube, cover tight reaction tube loam cake, reaction tube is put into the heating furnace flat-temperature zone again, the reaction tube charging temperature is controlled at below 200 ℃: setting the Heating Furnace Control temperature is 380 ℃, setting heating rate is 20 ℃/min, for preventing that the ferrous iron in the ore from reoxidizing, protect to the logical nitrogen of reaction tube with the flow of 3L/min, when temperature reaches 380 ℃, increase nitrogen flow to 10L/min, constant temperature 120min; Constant temperature takes out reaction tube after finishing in stove, continue to the logical nitrogen of reaction tube, and flow control is cooled to terminal temperature and stops logical nitrogen below 100 ℃ at 5L/min, opens the reaction tube loam cake, pours out sample, claims fixed its weight, is designated as m
1
According to formula
Calculate the water of crystallization percentage composition of the iron ore of this part sample.
Continue to take by weighing this sample according to the method described above and according to above-mentioned test condition revision test, carry out five groups of samples mensuration altogether, result of calculation is as shown in the table:
| Experiment is inferior | 1 | 2 | 3 | 4 | 5 | Mean value |
| Water of crystallization content (%) | 7.5 | 7.3 | 7.3 | 7.4 | 7.4 | 7.38 |
Through aforementioned calculation, drawing sample ore B water of crystallization content is 7.38%.
Execute example 3. and get sample ore C and put into baking box baking, 150 ℃ of baking temperatures, stoving time 60min takes out the back crushing screening, obtains
The sample of particle diameter.
Take by weighing 500g soil 0.1g sample, be designated as m
0Sample is inserted in the reaction tube, cover tight reaction tube loam cake, reaction tube is put into the heating furnace flat-temperature zone again, the reaction tube charging temperature is controlled at below 200 ℃: setting the Heating Furnace Control temperature is 430 ℃, setting heating rate is 25 ℃/min, for preventing that the ferrous iron in the ore from reoxidizing, protect to the logical nitrogen of reaction tube with the flow of 4L/min, when temperature reaches 400 ℃, increase nitrogen flow to 10L/min, constant temperature 30min when temperature reaches 430 ℃; Constant temperature takes out reaction tube after finishing in stove, continue to the logical nitrogen of reaction tube, and flow control is cooled to terminal temperature and stops logical nitrogen below 100 ℃ at 5L/min, opens the reaction tube loam cake, pours out sample, claims fixed its weight, is designated as m
1
According to formula
Calculate the water of crystallization percentage composition of the iron ore of this part sample.
Continue to take by weighing sample according to the method described above and according to above-mentioned test condition revision test, carry out seven groups of samples mensuration altogether, result of calculation is as shown in the table:
| Experiment is inferior | 1 | 2 | 3 | 4 | 5 | 6 | 7 | Mean value |
| Water of crystallization content (%) | 7.2 | 7.5 | 7.3 | 7.4 | 7.3 | 7.3 | 7.2 | 7.31 |
Through aforementioned calculation, drawing sample ore C water of crystallization content is 7.31%.
The inventive method also can be used for measuring fine ore water of crystallization content, and when measuring fine ore, the fine ore sample is put into stainless steel cup after mechanical water is removed in baking, again stainless steel cup is inserted reaction tube, and other step is identical with said process.
Claims (3)
1. an assay method that is used for iron ore crystal water content is characterized in that, it carries out according to following steps:
A. produce sample: need measure ore and put into the baking box baking, 100～150 ℃ of baking temperatures, stoving time 60～180min takes out the back crushing screening, obtains 10
12.5mm the sample of particle diameter;
B. sample is gone into stove: take by weighing 500g soil 0.1g sample, be designated as m
0, sample is inserted in the reaction tube, cover tight reaction tube loam cake, again reaction tube is put into heating furnace, the reaction tube charging temperature is controlled at below 200 ℃:
C. sample heating: sample heats in heating furnace, and setting the Heating Furnace Control temperature is 380
430 ℃, set heating rate less than 30 ℃/min, with 2
The flow of 10L/min is protected to the logical nitrogen of reaction tube, after temperature reaches controlling value, and constant temperature 30～120min;
D. sample cooling: constant temperature takes out reaction tube after finishing in stove, continues to the logical nitrogen of reaction tube, stops logical nitrogen below the cooling terminal temperature to 100 ℃, opens the reaction tube loam cake, pours out sample, claims fixed its weight, is designated as m
1
E. test findings is calculated:
W in the formula
JWater of crystallization percentage composition for the iron ore of this part sample;
F. this sample repeat above-mentioned b, c, d, e step 3 time, 5 times or 7 times, get the mean value of each time test findings, be the water of crystallization percentage composition of the ore of measuring.
2. the assay method that is used for iron ore crystal water content according to claim 1 is characterized in that: in the described sample heating steps when specimen temperature near or reach control during temperature, increase nitrogen flow to higher limit; In stove, take out reaction tube in the described sample cooling step, continue to lead to the flow control of nitrogen at 5L/min to reaction tube.
3. the assay method that is used for iron ore crystal water content according to claim 1 and 2 is characterized in that: described reaction tube is coke or ore hot performance test reaction tube, and described heating furnace is the reactive heating furnace of coke.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101968417A (en) * | 2010-09-02 | 2011-02-09 | 江西铜业股份有限公司 | Method for measuring volatile impurities in commercial molybdenum oxides pretreated by acid |
| CN102147347A (en) * | 2011-01-16 | 2011-08-10 | 首钢总公司 | Determination method for hydration rate curve of electrical steel dedicated magnesium oxide |
| CN102564886A (en) * | 2012-01-13 | 2012-07-11 | 河北钢铁股份有限公司唐山分公司 | Detection method for content of elemental calcium in alloy material for steelmaking |
| CN102590020A (en) * | 2012-03-06 | 2012-07-18 | 天津出入境检验检疫局化矿金属材料检测中心 | Method for determining free water weight in iron ore |
| CN102830035A (en) * | 2012-08-15 | 2012-12-19 | 四川鑫唐新能源科技有限公司 | Determination method for trace moisture content in positive electrode and negative electrode pole pieces of lithium battery |
| CN104692382A (en) * | 2014-12-10 | 2015-06-10 | 山东钢铁股份有限公司 | Method for preparing active carbon by using coke reactivity testing device |
| CN105181521A (en) * | 2015-09-07 | 2015-12-23 | 中国地质大学（北京） | Testing device and method for water content of shale |
| CN110243717A (en) * | 2019-06-20 | 2019-09-17 | 重庆科技学院 | It is a kind of for measuring the method and device of crystal water content in ore |
-
2008
- 2008-07-28 CN CNA2008100554774A patent/CN101329243A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101968417A (en) * | 2010-09-02 | 2011-02-09 | 江西铜业股份有限公司 | Method for measuring volatile impurities in commercial molybdenum oxides pretreated by acid |
| CN102147347A (en) * | 2011-01-16 | 2011-08-10 | 首钢总公司 | Determination method for hydration rate curve of electrical steel dedicated magnesium oxide |
| CN102564886A (en) * | 2012-01-13 | 2012-07-11 | 河北钢铁股份有限公司唐山分公司 | Detection method for content of elemental calcium in alloy material for steelmaking |
| CN102590020A (en) * | 2012-03-06 | 2012-07-18 | 天津出入境检验检疫局化矿金属材料检测中心 | Method for determining free water weight in iron ore |
| CN102830035A (en) * | 2012-08-15 | 2012-12-19 | 四川鑫唐新能源科技有限公司 | Determination method for trace moisture content in positive electrode and negative electrode pole pieces of lithium battery |
| CN104692382A (en) * | 2014-12-10 | 2015-06-10 | 山东钢铁股份有限公司 | Method for preparing active carbon by using coke reactivity testing device |
| CN104692382B (en) * | 2014-12-10 | 2017-01-18 | 山东钢铁股份有限公司 | Method for preparing active carbon by using coke reactivity testing device |
| CN105181521A (en) * | 2015-09-07 | 2015-12-23 | 中国地质大学（北京） | Testing device and method for water content of shale |
| CN105181521B (en) * | 2015-09-07 | 2016-08-17 | 中国地质大学（北京） | A kind of shale water content test device and method |
| CN110243717A (en) * | 2019-06-20 | 2019-09-17 | 重庆科技学院 | It is a kind of for measuring the method and device of crystal water content in ore |
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Open date: 20081224 |