CN103411989A - Analytical method for fly ash in blast furnace - Google Patents
Analytical method for fly ash in blast furnace Download PDFInfo
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- CN103411989A CN103411989A CN2013103242648A CN201310324264A CN103411989A CN 103411989 A CN103411989 A CN 103411989A CN 2013103242648 A CN2013103242648 A CN 2013103242648A CN 201310324264 A CN201310324264 A CN 201310324264A CN 103411989 A CN103411989 A CN 103411989A
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Abstract
The invention relates to an analytical method for fly ashes in a blast furnace. The method comprises the process steps of sample decarburization, melting, sample preparation, heating and sample measuring, and belongs to the field of chemical examination analysis of the blast furnace iron making. According to the invention, the method can accurately and quickly analyze the physical property and chemical ingredients of the fly ashes in blast furnace gas, accordingly, the use efficiency of blast furnace jetting powder coal is effectively improved, also the use efficiency of fly ashes in the blast furnace in the shaft furnace production process is improved, zero emission and environmental protection production are realized, and considerable economic benefits and social benefits are achieved.
Description
Technical field
The present invention relates to a kind of blast furnace dedusting ash analytical approach, belong to blast furnace ironmaking assay field.
Background technology
In the blast furnace process production run, in blast furnace gas, produce a large amount of dedusting ash, Iron Ore Powder, coke powder, vanadium titanium valve, lime stone, coal dust and auxiliary material etc. are arranged, for effectively instructing pulverized coal injection in blast furnace in dedusting ash, save coke, reduce pig iron cost and the use of dedusting ash in shaft furnace production.In the urgent need to exploring, seek a kind of method, carry out rapidly and accurately physical property and the chemical analysis analysis of dedusting ash in blast furnace gas, effectively in the service efficiency of raising pulverized coal injection in blast furnace and blast furnace gas, dedusting ash, in the use of shaft furnace production, is accomplished the environmental protection production of zero-emission.
Summary of the invention
In order to overcome above-mentioned deficiency, the present invention aims to provide a kind of blast furnace dedusting ash analytical approach, physical property and the chemical analysis analysis for the dedusting ash of the complicated crude fuel composition in blast furnace gas, not only can effectively detect fixed carbon in dedusting ash, and physical property and the chemical analysis analysis of the dedusting ash that the complicated crude fuel in blast furnace gas is formed have been realized, the smelting operation of shaft furnace brickmaking batching and shaft furnace production be can instruct, zero-emission and the environmental protection production of iron and steel enterprise realized.
Blast furnace dedusting ash analytical approach provided by the invention, quick and precisely carry out the sample carbon elimination to dedusting ash in blast furnace gas, the melting sample preparation, and heating, measure sample, specifically comprises the following steps:
(1) sample carbon elimination:
Take the dedusting ash sample (every square centimeter is no more than 0.15 gram) in cupel of 1.5000-2.0000 gram, cupel is sent in the horse resistance stove that temperature is no more than 100 ℃, fire door stays the gap of 15mm left and right, be warming up to 500 ℃, keep 30min, rise to 815 ± 15 ℃, calcination is 2 hours at this temperature, takes out cooling in exsiccator;
(2) melting sample preparation
In platinum crucible, accurately take the high-purity lithium tetraborate of 6.000 ± 0.001 gram, sample 0.5000 ± 0.0002 gram, then take 0.6000 ± 0.0002 gram sodium nitrate, in 0.6000 gram ± 0.0002 gram cobalt, mark, add 0.030 gram lithium bromide as remover in platinum crucible;
(3) heating
Platinum yellow gold crucible is placed on the melting furnace tripod, after device initialize, selects type of heating, 1200 ℃ of design temperatures, the molten 420 seconds sample time, spin and revolution were waved 420 seconds, heated, mixed in cooling 360 seconds, eliminated sample particle and mineral effect;
(4) measure sample
1. after melting, the platinum alloy crucible is taken out, make homogeneous glass sheet sample, wherein be close to platinum crucible and simultaneously be measurement face;
2. x-ray fluorescence analyzer setting parameter:
X-ray tube voltage: 50kV, electric current: 50mA
Analysis room's vacuum tightness: high vacuum 8 Pa
The x-ray bombardment time: 40s
Sample box: spin 60 rev/mins
Select element: Fe, Si, Ca, Mg, Al, P
The PHA(pulse height is set regulates): 100-300;
The peak position of Wave Height Distribution curve can slowly change after long-time, it is exactly that departing from of peak position adjusted to processing that PHA regulates;
3. set up analytic curve:
Select the standards for iron ore sample of the different gradients of each component, set up analytic curve;
4. blast furnace dedusting ash glass sheet sample, put into x-ray fluorescence analyzer sample boxlike, selects analysis of iron ore;
(5) precision analysis: according to analytical approach and instrumental analysis condition that experiment is set, after 11 calcination carbon eliminations of same sample repetition, the fuse piece of preparation is measured, and result shows that the precision of measurement result is good, meets and analyzes requirement.
In above-mentioned analytical approach, be designated as in cobalt: Li
2B
4O
7: in CoO=9:1, Co, mark is as in Fe K β line, marking.
The pre-service of described sample: under 108 ℃, dried 40 minutes, exsiccator claims sample after cooling 5 minutes again.
In technical solution of the present invention, be mixed with the sample forbidding platinum crucible of the elements such as metal simple-substance and carbon.
The analytical approach of blast furnace dedusting ash provided by the invention, unlike the prior art be, at first having carried out the sample carbon elimination processes, the sample carbon elimination not only can effectively detect the fixed carbon in dedusting ash, and can play certain directive significance to blast furnace production, reach the purpose of efficiently utilizing dedusting ash, realized environmental protection production.
Of the present invention
Beneficial effect:
By to the blast furnace dedusting ash analysis, first can effectively detect fixed carbon in dedusting ash, can instruct blast furnace to improve and adjust the blast furnace process operation, effectively improves the burning efficiency of coal injection; Physical property and the chemical analysis analysis of the dedusting ash that the complicated crude fuel in the second pair of blast furnace gas forms, can instruct the smelting operation of shaft furnace brickmaking batching and shaft furnace production, realizes zero-emission and the environmental protection production of iron and steel enterprise.
Embodiment
Below by embodiment, further illustrate the present invention, but be not limited to following examples.
Embodiment: the analytical approach of blast furnace dedusting ash
The present embodiment comprises the sample carbon elimination, the melting sample preparation, and heating, measure sample, specifically comprises the following steps:
(1) sample carbon elimination:
Take the dedusting ash sample (every square centimeter is no more than 0.15 gram) in cupel of 2.0000 grams, cupel is sent in the horse resistance stove that temperature is no more than 100 ℃, fire door stays the gap of 15mm left and right, be warming up to 500 ℃, keep 30min, rise to 815 ± 15 ℃, calcination is 2 hours at this temperature, takes out cooling in exsiccator;
(2) melting sample preparation
In platinum crucible, accurately take the high-purity lithium tetraborate of 6.000 ± 0.001 gram, sample 0.5000 ± 0.0002 gram, then take 0.6000 ± 0.0002 gram sodium nitrate, in 0.6000 gram ± 0.0002 gram cobalt, mark, add 0.030 gram lithium bromide as remover in platinum crucible;
(3) heating
Platinum yellow gold crucible is placed on the melting furnace tripod, after device initialize, selects type of heating, 1200 ℃ of design temperatures, the molten 420 seconds sample time, spin and revolution were waved 420 seconds, heated, mixed in cooling 360 seconds, eliminated sample particle and mineral effect;
(4) measure sample
1. after melting, the platinum alloy crucible is taken out, make homogeneous glass sheet sample, wherein be close to platinum crucible and simultaneously be measurement face;
2. x-ray fluorescence analyzer setting parameter:
X-ray tube voltage: 50kV, electric current: 50mA
Analysis room's vacuum tightness: high vacuum 8 Pa
The x-ray bombardment time: 40s
Sample box: spin 60 rev/mins
Select element: Fe, Si, Ca, Mg, Al, P
PHA:100-300 is set;
3. set up analytic curve:
At first select standards for iron ore sample 13709,15707,30006-93,30002,13711,31006,30004,31005,30003,11701, W-7177,93-40, the 93-97,01042,01015 of the different gradients of each component, set up analytic curve;
Iron ore curve each component related coefficient: Fe-KB 9.98457e-001, Si-KA 9.99789 e-001, Ca-KA 9.97671 e-001, Mg-KA 9.97025 e-001, Al-KA 9.90971 e-001, P-KA 9.96138 e-001, the infrared oscillometry of S;
4. blast furnace dedusting ash glass sheet sample, put into x-ray fluorescence analyzer sample boxlike, selects analysis of iron ore.
(5) precision analysis:
According to analytical approach and instrumental analysis condition that experiment is set, after 11 calcination carbon eliminations of same sample repetition, the fuse piece of preparation is measured, and result shows that the precision of measurement result is good, meets and analyzes requirement, and analysis result is in Table 1.
Table 1 pair same sample repeats the precision analysis of 11 calcination results
Simultaneously, the blast furnace dedusting ash that the present embodiment is related to carries out chemical analysis, the results are shown in Table 2 to component analysis; The average of chemical analysis results and xrf analysis result is made comparisons, and analyzes according to standard GB/T 6730.5-2007, YB506-65, and the data that two kinds of analytical approachs draw are within the permissible error scope.
Two kinds of methods and resultses of table 2 relatively
Claims (3)
1. blast furnace dedusting ash analytical approach, it is characterized in that: comprise sample carbon elimination, melting sample preparation, heating, measurement sample technique, concrete steps are:
(1) sample carbon elimination:
Take the dedusting ash sample of 1.5000-2.0000 gram in cupel, every square centimeter is no more than 0.15 gram, cupel is sent in the horse resistance stove that temperature is no more than 100 ℃, fire door stays the gap of 15mm, be warming up to 500 ℃, keep 30min, rise to 815 ± 15 ℃, calcination is 2 hours at this temperature, takes out cooling in exsiccator;
(2) melting sample preparation
In platinum crucible, accurately take the high-purity lithium tetraborate of 6.000 ± 0.001 gram, sample 0.5000 ± 0.0002 gram, then take 0.6g ± 0.0002 gram sodium nitrate, in 0.6000 gram ± 0.0002 gram cobalt, mark, add 0.030 gram lithium bromide as remover in platinum crucible;
(3) heating
Platinum yellow gold crucible is placed on the melting furnace tripod, after device initialize, selects type of heating, 1200 ℃ of design temperatures, the molten 420 seconds sample time, spin and revolution were waved 420 seconds, heated, mixed in cooling 360 seconds, eliminated sample particle and mineral effect;
(4) measure sample
1. after melting, the platinum alloy crucible is taken out, make homogeneous glass sheet sample, wherein be close to platinum crucible and simultaneously be measurement face;
2. x-ray fluorescence analyzer setting parameter:
X-ray tube voltage: 50kV, electric current: 50mA
Analysis room's vacuum tightness: high vacuum 8 Pa
The x-ray bombardment time: 40s
Sample box: spin 60 rev/mins
Select element: Fe, Si, Ca, Mg, Al, P
Pulse height is set regulates: 100-300;
3. set up analytic curve:
Select the standards for iron ore sample of the different gradients of each component, set up analytic curve;
4. blast furnace dedusting ash glass sheet sample, put into x-ray fluorescence analyzer sample boxlike, selects analysis of iron ore.
2. blast furnace dedusting ash analytical approach according to claim 1, is characterized in that: in described step (2) melting sample preparation, in cobalt, mark and meet: Li
2B
4O
7: in CoO=9:1, Co, mark is as in Fe K β line, marking.
3. blast furnace dedusting ash analytical approach according to claim 1, it is characterized in that: described sample need pass through pre-service: under 108 ℃, dried 40 minutes, exsiccator claims sample after cooling 5 minutes again.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758671A (en) * | 2015-07-24 | 2016-07-13 | 解海龙 | Method for adjusting sampling quantity in real time during automatic sampling of ash outlet of dry collector |
| CN105925740A (en) * | 2016-06-22 | 2016-09-07 | 北京科技大学 | Optimization method of converter fly ash for blast furnace blowing |
| CN107102096A (en) * | 2017-06-12 | 2017-08-29 | 常州第六元素材料科技股份有限公司 | Graphene oxide content of ashes detection method |
| CN108982562A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | The preparation method of cobalt internal standard XRF analysis sheet glass based on assisted ejection agent |
| CN109580326A (en) * | 2018-12-05 | 2019-04-05 | 西王金属科技有限公司 | The measuring method of zinc oxide and alkali metal in a kind of dedusting ash |
| CN110376230A (en) * | 2019-08-13 | 2019-10-25 | 凉山矿业股份有限公司 | The method of X-ray fluorescence spectra analysis boiler smoke Cu, As, Pb, Zn element |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758671A (en) * | 2015-07-24 | 2016-07-13 | 解海龙 | Method for adjusting sampling quantity in real time during automatic sampling of ash outlet of dry collector |
| CN105758671B (en) * | 2015-07-24 | 2018-12-18 | 解海龙 | Adjust the method for sampling quantity in real time when dry collector ash hole samples automatically |
| CN105925740A (en) * | 2016-06-22 | 2016-09-07 | 北京科技大学 | Optimization method of converter fly ash for blast furnace blowing |
| CN107102096A (en) * | 2017-06-12 | 2017-08-29 | 常州第六元素材料科技股份有限公司 | Graphene oxide content of ashes detection method |
| CN107102096B (en) * | 2017-06-12 | 2019-12-13 | 常州第六元素材料科技股份有限公司 | Method for detecting ash content of graphene oxide |
| CN108982562A (en) * | 2018-08-03 | 2018-12-11 | 武汉科技大学 | The preparation method of cobalt internal standard XRF analysis sheet glass based on assisted ejection agent |
| CN108982562B (en) * | 2018-08-03 | 2021-02-19 | 武汉科技大学 | Preparation method of cobalt internal standard XRF (X-ray fluorescence) analysis glass sheet based on release assisting agent |
| CN109580326A (en) * | 2018-12-05 | 2019-04-05 | 西王金属科技有限公司 | The measuring method of zinc oxide and alkali metal in a kind of dedusting ash |
| CN110376230A (en) * | 2019-08-13 | 2019-10-25 | 凉山矿业股份有限公司 | The method of X-ray fluorescence spectra analysis boiler smoke Cu, As, Pb, Zn element |
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Application publication date: 20131127 |