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Fusion preparation method of vanadium-iron alloy fuse piece

A technology for vanadium ferroalloy and flakes, which is applied in the field of melting and preparation of vanadium ferroalloy flakes, can solve the problems of slow reaction and evaporation speed, many residual residues, low efficiency, etc., achieves elimination of mineral effect and particle size effect, and solves difficult oxidation of alloys. , the effect of high efficiency

Inactive Publication Date: 2019-08-16
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Application Information

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Problems solved by technology

The main problems of this method are: 1. Nitric acid should be added dropwise during acid dissolution, and then sulfuric acid should be added dropwise. The dissolution and evaporation temperature should be controlled to be less than 100°C, otherwise the sample reacts violently and splashes, resulting in the loss of the element to be measured; 2. 1. The reaction and evaporation speed is slow, time-consuming, and low in efficiency; 3. For the vanadium-iron sample with a silicon content exceeding 2%, it cannot be completely decomposed, and there are many residual residues. The undecomposed alloy sample corrodes the crucible during the second step of flux melting
This invention is also carried out in the platinum gold crucible. The operating conditions are harsh, and a slight mistake will cause the platinum gold crucible to corrode and cause irreparable losses.
[0007] CN102207475A discloses a metal alloy X-ray fluorescence spectrum detection method using a new sample preparation technology, which also adopts acid dissolution, then adds alkali to precipitate the element to be measured, filters the precipitate, and the precipitate is dried, carbonized, ashed, and ignited. Burning and other steps to convert the residue into metal oxides, and calculate the weight of the residue, and finally melt the burned residue, this method is very cumbersome to operate, and is not suitable for V, Si, Mn, P, Al in ferrovanadium Simultaneous determination of
This method is simple, but the details of the operation are particularly critical. Pre-oxidation conditions, temperature, flux ratio and other conditions are not controlled precisely enough, which will cause the sample to splash out of the crucible during pre-oxidation, and the incomplete pre-oxidation of alloy elements will corrode the crucible. The key lies in the choice of control conditions

Method used

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  • Fusion preparation method of vanadium-iron alloy fuse piece
  • Fusion preparation method of vanadium-iron alloy fuse piece
  • Fusion preparation method of vanadium-iron alloy fuse piece

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preparation example Construction

[0026] The melting preparation method of vanadium-iron alloy melting piece of the present invention comprises the following steps:

[0027] a: Raw material preparation, weigh 3-4 parts by weight of lithium tetraborate as the main flux, 1 part by weight of lithium carbonate as the flux, 0.5-1 part by weight of oxidant and 0.1 part by weight of the sample in a filter paper bag, mix Uniform, wrapped into a ball;

[0028] b. Sample pre-oxidation, put the filter paper bag wrapped into a spherical shape in step a into a porcelain crucible with graphite powder as the bottom, place the porcelain crucible in a muffle furnace with a temperature not higher than 200°C, and heat up through the following program for melting Pre-oxidation: The heating time of the first step is not less than 20 minutes, from the initial temperature to 600°C ± 10°C; 1000℃~1100℃±10℃ holding time is not less than 15min; in the third step, the cooling time is not less than 20min, and the porcelain crucible is ta...

Embodiment 1

[0041] The determination of the amount of vanadium, silicon, aluminum, manganese and phosphorus in ferrovanadium is carried out by the following steps:

[0042] (1) The preparation of vanadium-iron glass frit is completed through the following steps

[0043] A. Accurately weigh 6.0000g of lithium tetraborate, 1.5000g of lithium carbonate, and 0.1500g of ferrovanadium sample in a filter paper bag, add about 0.7 ammonium nitrate, mix the analysis flux and the sample in the filter paper bag evenly, and wrap it into a spherical shape ;

[0044] B. Put the filter paper bag wrapped into a spherical shape into the porcelain crucible with graphite powder as the bottom in advance, put it into the muffle furnace, turn on the power supply of the muffle furnace, and set the sample pre-oxidation temperature. The procedure is as follows: the heating time of the first working step is 30min, the initial temperature rises from room temperature 25°C to 600°C (±10°C); the heating time of the se...

Embodiment 2

[0058] The determination of the amount of vanadium, silicon, aluminum, manganese and phosphorus in ferrovanadium is carried out by the following steps:

[0059] (1) The preparation of vanadium-iron glass frit is completed through the following steps

[0060] A. Accurately weigh 6.5000g of lithium tetraborate, 1.5000g of lithium carbonate, and 0.2000g of ferrovanadium sample in a filter paper bag, add about 1.5g of ammonium nitrate, mix the analysis flux and the sample in the filter paper bag, and wrap it into spherical

[0061] B. Put the filter paper bag wrapped into a spherical shape into the porcelain crucible with graphite powder as the bottom in advance, put it into the muffle furnace, turn on the power supply of the muffle furnace, and set the sample pre-oxidation temperature. The procedure is as follows: the heating time of the first working step is 20min, the initial temperature rises from 150°C to 600°C (±10°C); the heating time of the second step is 90min, the tempe...

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Abstract

The invention discloses a fusion preparation method of a vanadium-iron alloy fuse piece in the technical field of metal analysis and detection. The fusion preparation method comprises the following steps of firstly, weighing a certain amount of lithium tetraborate, lithium carbonate, an oxidizing agent and a test material in a filtering paper bag, performing uniform mixing, and wrapping to form aspherical shape; secondly, placing the raw materials in a porcelain crucible taking graphite powder as a substrate in advance, and performing pre-oxidization on the raw materials by a two-step temperature rising and one-step temperature reduction method; and finally, placing the raw materials in a platinum gold crucible to fabricate a glass sheet to be measured. The fusion preparation method has the beneficial effects that by application of a main solvent and the oxidizing agent in a matching way and by scientific design of a fusion temperature and fusion rate, the vanadium-iron alloy sample is completely pre-oxidized, the fused sample is uniform, has no bubbles and is not broken, and main and secondary elements are good in measurement accuracy and high in accuracy.

Description

technical field [0001] The invention relates to the technical field of metal analysis and detection, in particular to a melting preparation method of vanadium-iron alloy melting pieces. Background technique [0002] Vanadium ferroalloy is an important raw material for steelmaking to improve the process and performance of steel. The product standard GB / T4139-2012 has clear requirements for the content of primary and secondary elements V, Si, P, Al, and Mn of each brand, so accurate analysis The primary and secondary components in ferrovanadium are an important link in controlling the quality of steel. At present, the classic method for determining the content of elements in vanadium-iron alloy is the national standard, that is, the ferrous ammonium sulfate titration method and the potentiometric titration method (GB / T8704.5-2007) are used to determine the V element content, and the chrome azure S spectrophotometric method and EDTA titration Method (GB / T 8704.8-2009) to deter...

Claims

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Application Information

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IPC IPC(8): G01N23/2202
CPCG01N23/2202
Inventor 郑小敏於利慧
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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