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Method for detecting trace metal elements in coke and application thereof

A technology of trace metal elements and detection methods, which is applied in the field of chemical analysis, can solve problems such as lack of detection methods, abnormal furnace conditions, and impact on coke quality, and achieve the effects of meeting acceptance requirements, improving accuracy, and strong operability

Active Publication Date: 2020-01-10
YANGCHUN NEW STEEL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is also a lack of detection methods for trace metal elements in coke in the industry, and in the coking plant, due to desulfurization waste liquid, residual ammonia water in the coking process, denitrification waste liquid, scaling washing water of power generation boilers, biochemical dephenolization water, etc. directly enter the coke quenching pool , participate in the water coke quenching operation, the complex process leads to the final coke containing a variety of metal elements, which affects the quality of the coke
Most of the detection technologies for coke in the prior art only focus on the detection of soluble metal ions on the surface of coke, but do not propose an accurate and quantitative detection technology for the total content of specific trace metal elements in coke
[0003] Coke is widely used as smelting fuel in metallurgical enterprises. Coke containing a variety of trace metal elements such as K, Na, Ca, Mg, and Zn, after the metal ions are vaporized after being heated in the upper part of the blast furnace, the carbon dissolution loss of coke will react positively. Catalysis, that is, to promote the gasification reaction of charcoal, resulting in a decrease in coke strength, thereby weakening the skeleton role of coke in the blast furnace, and the enrichment of some metal ions in the blast furnace will aggravate the disastrous expansion and majority sintering of pellets Medium-temperature reduction pulverization of ore, lower iron ore reflow temperature, etc., resulting in poor air permeability of blast furnace, increased pressure difference, fluctuations in furnace conditions and even abnormal furnace conditions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A sample pretreatment method for the determination of trace metal elements in coke, comprising the following steps:

[0030] (1) Take the coke sample that enters the factory and crush it step by step through a 13mm sieve, take 2kg of sieved coke and soak it in water to prepare the coke sample; stir the sample evenly, weigh the sample according to Table 1 and place it in a 3000ml beaker, Add 1000ml deionized water, stir well and let it stand for more than 3 hours;

[0031] (2) Stir and mix the coke soaking solution, and then use slow quantitative filter paper to filter the soaked coke soaking solution to ensure that there are no visible particles in the filtrate;

[0032] (3) Get filtrate in the volumetric flask of 50ml, constant volume, add concentration again and be 50% nitric acid solution 1ml, mix to obtain the first mixed solution, promptly obtain the part metal ion solution in the coke to be measured.

Embodiment 2

[0034] A kind of detection method of calcium, magnesium content in coke, comprises the following steps: step (1)-(3) is identical with embodiment 1, also comprises the steps:

[0035] Take 1.0g of filter residue and dry it at low temperature, place it in a porcelain crucible, put it into a muffle furnace, and burn it at 400°C for 1.5h, 480°C for 2h, and finally at 550°C for 1.5h according to the set heating program. ". After the heating program is over, take it out and place it at room temperature, transfer it to a tetrafluoroethylene beaker with a small amount of water, add 10mL of hydrofluoric acid, 5.0mL of aqua regia and 1.5mL of perchloric acid in sequence, and slowly raise the temperature to 280°C on the electric heating plate. After the fumes of perchloric acid are exhausted, lower the temperature, add 1ml of nitric acid solution with a concentration of 50% to extract the sample, cool to room temperature, transfer the solution into a 50mL polytetrafluoroethylene volumet...

Embodiment 3

[0037] The contents of calcium and magnesium ions in the first mixed solution and the second mixed solution were respectively detected by EDTA titration.

[0038] The above technical scheme prepares a representative coke sample, soaks it in deionized water for several hours, prepares a solution to be tested, and uses GB / T 15452-2009 "Determination of Calcium and Magnesium Ions in Industrial Circulating Cooling Water by EDTA Titration Method" to measure The content of calcium and magnesium in the solution to be tested solves the technical problem that the content of adsorbed calcium and magnesium in coke cannot be detected at present.

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PUM

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Abstract

The invention discloses an extraction method of trace metal elements in coke and an application. The extraction method comprises the following steps: taking coke to prepare a sample, uniformly stirring the sample, weighing the sample, putting the sample into a beaker, adding deionized water, performing uniform stirring, and standing for a plurality of hours; filtering the soaked coke soak solutionto ensure that no visible particulate matters exist in the filtrate; adding the filtrate into a volumetric flask, fixing the volume, adding a nitric acid solution, and performing uniform mixing to obtain a first to-be-detected solution; and drying the filter residues, performing ashing, carrying out mixed acid digestion treatment to obtain a second to-be-detected solution; and finally, respectively measuring the content of the target metal element by adopting an EDTA method and an inductively coupled plasma atomic emission spectrometry. The method can extract the metal elements in the coke, has the advantages of simple steps, short time consumption and high extraction efficiency, and can eliminate experiment interference by adopting deionized water.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a detection method and application of trace metal elements in coke. Background technique [0002] Most of the domestic long-process iron and steel complexes are equipped with coking plants. Generally, a large proportion or even all of them use self-produced coke, and the quality is relatively stable and controllable. The problem of trace metal elements in coke has attracted enough attention. There is also a lack of detection methods for trace metal elements in coke in the industry, and in the coking plant, due to desulfurization waste liquid, residual ammonia water in the coking process, denitrification waste liquid, scaling washing water of power generation boilers, biochemical dephenolization water, etc. directly enter the coke quenching pool , Participate in water coke quenching operations, the complex process leads to the final coke containing a variety of metal el...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N21/73G01N1/28G01N1/44
CPCG01N1/28G01N1/44G01N21/73G01N31/16
Inventor 樊尧桂程祥刘林刚郑呈祥周小盛刘涛
Owner YANGCHUN NEW STEEL CO LTD
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