CN111122562A - Method for determining TFe content in steel slag magnetic separation powder - Google Patents
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Abstract
The invention discloses a method for determining TFe content in steel slag magnetic separation powder, belonging to the technical field of analysis and detection. The method disclosed herein uses a closed grinder to process the steel slag magnetic separation powder into powder, screens the powder, then uses a magnet block to absorb magnetic substances in oversize products, all the rest samples are prepared into analysis samples with the granularity of 120 meshes, then uses a chemical method to analyze the TFe content in the oversize products and the analysis samples with the granularity of 120 meshes, and then can accurately calculate the TFe content in the steel slag magnetic separation powder according to the weight, thereby being capable of effectively guiding the smelting production of a steel mill.
Description
Technical Field
The invention belongs to the technical field of analysis and detection, relates to a method for determining TFe content in steel slag magnetic separation powder, and particularly relates to a method for determining TFe content in steel slag magnetic separation powder with the TFe content range of 15% -35%.
Background
The steel slag is one of the main sources of the solid wastes of the steel enterprises, and the reasonable utilization of the steel slag can reduce the pollution of the solid wastes to the environment and the resource waste. The steel slag as a secondary resource is comprehensively utilized in two main ways, one way is that the steel slag is used as a smelting flux to be recycled in the factory, the steel slag not only can replace limestone, but also can recover a large amount of iron and other useful elements from the limestone, and the other way is that the steel slag is used as a road building material or a raw material of agricultural fertilizer.
As the steel slag recycled for steel mill smelting has low iron content and low use value, the steel slag is processed into the steel slag magnetic separation powder with the content of 15-35 percent, and can be effectively utilized in the steel mill smelting process.
Due to the limitation of the process, magnetic substances and non-magnetic substances in the prepared steel slag magnetic separation powder are often wrapped together and cannot be effectively separated, so that certain difficulty is caused in the subsequent accurate analysis of the TFe content in the steel slag magnetic separation powder, and therefore, an analysis means with high accuracy is urgently needed to determine the TFe content in the steel slag magnetic separation powder so as to effectively guide the smelting production of a steel mill.
Disclosure of Invention
Aiming at one or more problems in the prior art, the invention provides a method for measuring TFe content in steel slag magnetic separation powder, which comprises the following steps:
1) quantitatively weighing steel slag magnetic separation powder as a sample to be detected, and recording the mass as m0；
2) Grinding, crushing and screening the sample to be detected to obtain a first oversize product and a first undersize product;
3) and (3) absorbing the magnetic wrappage on the first oversize product by using a magnet until the magnetic wrappage is completely absorbed, taking the absorbed magnetic wrappage as a second detection sample, and recording the mass as m2And the other first oversize products are used as second oversize products;
4) grinding, crushing and screening the second oversize product again to obtain a second undersize product, mixing the second undersize product with the first undersize product to serve as a first detection sample, and recording the mass as m1And m is1＝m0-m2；
5) Respectively measuring the TFe content in the first detection sample and the second detection sample by adopting a chemical analysis method;
6) and (4) calculating the TFe content in the steel slag magnetic separation powder.
In the method, the granularity of the steel slag magnetic separation powder in the step 1) is 10-15 mm, and the TFe content is 15-35%.
In the method, in the step 2), a closed grinder is used for grinding and crushing the sample to be detected, and then a 120-mesh square-hole sieve is used for sieving to obtain a first oversize product and a first undersize product.
In the above method, the specific operation method of sucking the magnetic package from the first oversize material by the magnet in the step 3) is as follows: and (4) sucking the magnetic wrappage on the first oversize product by using a paper wrapped magnet until the magnetic wrappage is completely sucked.
In the method, the second oversize product in the step 4) is ground, crushed and sieved again by using an internal crusher, and then all the second oversize product is sieved by using a 120-mesh square-hole sieve.
In the above method, the specific operation steps of determining the content of TFe in the first test sample and the second test sample by using a chemical analysis method in step 5) are as follows:
6.1, quantitatively weighing a sample in a 300mL triangular flask, adding 20mL sulfuric acid-phosphoric acid mixed acid, dissolving the mixture on a high-temperature electric furnace until sulfuric acid fume leaves the bottom of the flask to the height of one half of the flask, taking down the flask for slight cooling, adding 20mL hydrochloric acid (1+1), reducing the mixture to light yellow by using a 60g/L tin dichloride solution, taking down the flask for slight cooling, and adding 50mL hot water to keep the temperature of the solution at 40-50 ℃;
6.2, adding 8 drops of sodium tungstate solution with the concentration of 250g/L, reducing the solution to stable blue by using titanium trichloride solution (1+9), dripping potassium dichromate standard solution with the concentration of 0.05mol/L until the blue disappears, immediately adding four drops of diphenylamine sodium sulfonate solution with the concentration of 4g/L, titrating the potassium dichromate standard solution with the concentration of 0.05mol/L to stable purple as an end point, recording the volume (mL) of the titration, synchronously adopting a blank reagent as a control, and calculating the content of TFe in the sample by using the following formula:
in the formula:
V0: volume of potassium dichromate standard titration solution (mL) consumed for blank reagents;
v: volume (mL) of potassium dichromate standard titration solution consumed by the sample;
c: concentration (mol/L) of potassium dichromate standard titration solution;
m: sample mass (g);
m: molar mass of iron (55.85 g/mol);
wherein the TFe content in the obtained first test sample is W (TFe)1) (%), the TFe content in the second test sample was W (TFe)2)(％)。
In the above method, the preparation method of the sulfuric acid-phosphoric acid mixed acid in step 6.1 is: slowly injecting 150mL of sulfuric acid with the concentration of 1.84g/mL into 700mL of water under stirring, cooling, then adding 150mL of phosphoric acid with the concentration of 1.70g/mL, and uniformly mixing;
the preparation method of the titanium trichloride solution in the step 6.2 comprises the following steps: 1 part of titanium trichloride solution with the mass concentration of 15-20% is transferred and added with 9 parts of hydrochloric acid (1+3) to be mixed evenly.
In the method, the formula for calculating the TFe content in the steel slag magnetic separation powder in the step 6) is as follows:
W(TFe)(％)＝(m1×W(TFe1)(％)+m2×W(TFe2)(％))/m0
wherein:
m0the mass (g) of a sample to be detected;
m1is the first test sample mass (g), i.e., m0-m2；
m2Is the second test sample mass (g);
W(TFe1) (%) represents the content of TFe in the first test sample;
W(TFe2) (%) represents the content of TFe in the second test sample;
w (tfe) (%): and (4) determining the TFe content in the sample to be tested.
The method for determining the TFe content in the steel slag magnetic separation powder provided by the technical scheme comprises the steps of processing the steel slag magnetic separation powder into powder by using a closed crusher, screening, absorbing magnetic substances in oversize products by using a magnet block, preparing all residual samples into analysis samples with the granularity of 120 meshes, wherein the granularity of 120 meshes can meet the uniformity and the representativeness of the analysis samples, analyzing the TFe content in the oversize products and the analysis samples with the granularity of 120 meshes by using a chemical method, accurately calculating the TFe content in the steel slag magnetic separation powder according to the weight, and effectively guiding a steel mill to smelt and produce.
Detailed Description
Because the steel slag magnetic separation powder contains TFe, if a conventional method for directly carrying out chemical analysis is adopted for grinding to prepare an analysis sample, metal particles in the steel slag magnetic separation powder can be flaky or have larger and larger volume along with the extension of grinding time, the particle size of the metal particles cannot be reduced by a grinding means, and the particle size of other components can be reduced along with the extension of the grinding time, so that the uneven particle size distribution of the sample can be caused by grinding the steel slag magnetic separation powder, an effective analysis sample is difficult to obtain, and great obstacle is caused to the determination of the content of TFe in the steel slag magnetic separation powder. The invention overcomes the obstacles of the prior art and obtains a method capable of accurately detecting the TFe content in the steel slag magnetic separation powder.
The present invention will be described in detail with reference to the following specific embodiments.
The embodiments are provided for the detailed implementation and the specific operation process, which will help to understand the present invention, but the scope of the present invention is not limited to the following embodiments.
Example 1:
1) uniformly mixing steel slag magnetic separation powder with the granularity of 10-15 mm and the weight of about 2.5kg by a stacking method, gradually dividing by a quartering method, taking a sample as a sample to be detected, accurately weighing 100g of the sample, and recording as m0Accurate to 0.1 g;
2) dividing 100g of a weighed sample to be detected into two times, grinding and crushing the two times in a closed crusher for 300s, and after the 100g of the sample is completely treated, screening the sample by using a 120-mesh square-hole sieve to obtain a first oversize product and a first undersize product;
3) absorbing the magnetic wrappage in the first oversize material for 2-3 times by using a paper wrapped magnet block until the magnetic wrappage is completely absorbed, taking the absorbed magnetic wrappage as a second detection sample, weighing to obtain a mass of 31.3g, recording the mass as m2Accurate to 0.1 g;
4) grinding and crushing the first oversize product which is not sieved completely after the absorbed magnetic wrappage in a closed crusher again, sieving the first oversize product by using a 120-mesh square-hole sieve until the first oversize product is sieved completely, combining and uniformly mixing the undersize product and the first undersize product in the step 2) to serve as a first detection sample, wherein the mass of the first inspection sample is (m)0-m2)68.7g, is recorded as m1；
5) Weighing 0.2000g of analysis sample in the first detection sample and 0.9987g of analysis sample in the second detection sample, and respectively determining by adopting a chemical analysis method to obtain the TFe contents of 18.90% and 34.50% in the first detection sample and the second detection sample respectively; the chemical analysis method comprises the following steps: quantitatively weighing a sample in a 300mL triangular flask, adding 20mL sulfuric acid-phosphoric acid mixed acid (150 mL sulfuric acid with the concentration of 1.84g/mL is slowly injected into 700mL water under stirring, adding 150mL phosphoric acid with the concentration of 1.70g/mL after cooling, uniformly mixing), dissolving on a high-temperature electric furnace until sulfuric acid fume leaves the bottom of the flask to a half of the height of the flask, taking down the flask for slight cooling, adding 20mL hydrochloric acid (1+1), reducing the solution to light yellow by using a tin dichloride solution with the concentration of 60g/L, taking down the flask for slight cooling, and adding 50mL hot water to keep the temperature of the solution at 40-50 ℃; adding 8 drops of sodium tungstate solution with the concentration of 250g/L, reducing the solution to stable blue by using titanium trichloride solution (1+9) (transferring 1 part of titanium trichloride solution with the mass concentration of 15-20%, adding 9 parts of hydrochloric acid (1+3), uniformly mixing the solution and the solution), dripping potassium dichromate standard solution with the concentration of 0.05mol/L until the blue disappears, immediately adding four drops of diphenylamine sodium sulfonate solution with the concentration of 4g/L, titrating the solution to stable purple by using the potassium dichromate standard solution with the concentration of 0.05mol/L, recording the volume (mL) of the titration, synchronously using a blank reagent as a control, and calculating the content of TFe in the sample by using the following formula:
in the formula:
V0: volume of potassium dichromate standard titration solution (mL) consumed for blank reagents;
v: volume (mL) of potassium dichromate standard titration solution consumed by the sample;
c: concentration (mol/L) of potassium dichromate standard titration solution;
m: sample mass (g);
m: molar mass of iron (55.85 g/mol);
wherein the TFe content in the obtained first test sample is W (TFe)1) (%), the TFe content in the second test sample was W (TFe)2)(％)；
6) Calculating the TFe content in the steel slag magnetic separation powder according to the weight;
the calculation formula of the analysis result is as follows:
W(TFe)(％)＝(m1×W(TFe1)(％)+m2×W(TFe2)(％))/m0
＝(68.7×18.90％+31.3×34.50％)/100＝23.8％
in the formula:
m0: the total mass (g) of the sample to be tested;
m1: a mass (g) of the first test sample;
m2: mass (g) of the second test sample;
W(TFe1) (%): the TFe content in the first detection sample;
W(TFe2) (%): the TFe content in the second detection sample;
w (tfe) (%): TFe content in a sample to be detected;
the TFe content in the obtained steel slag magnetic separation powder is 23.8 percent by calculation.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for measuring TFe content in steel slag magnetic separation powder is characterized by comprising the following steps:
1) quantitatively weighing steel slag magnetic separation powder as a sample to be detected, and recording the mass as m0；
2) Grinding, crushing and screening the sample to be detected to obtain a first oversize product and a first undersize product;
3) and absorbing the magnetic wrappage on the first oversize product by using a magnet until the magnetic wrappage is completely absorbed, taking the absorbed magnetic wrappage as a second detection sample, and recording the mass as m2And the other first oversize products are used as second oversize products;
4) grinding, crushing and screening the second oversize product again to obtain a second undersize product, mixing the second undersize product with the first undersize product to serve as a first detection sample, and recording the mass as m1And m is1＝m0-m2；
5) Respectively measuring the TFe content in the first detection sample and the second detection sample by adopting a chemical analysis method;
6) and (4) calculating the TFe content in the steel slag magnetic separation powder.
2. The method as claimed in claim 1, wherein the steel slag magnetic separation powder in the step 1) has a particle size of 10mm to 15mm and a TFe content of 15% to 35%.
3. The method as claimed in claim 1, wherein the sample to be tested is ground and pulverized in step 2) by using a closed type pulverizer, and then sieved by using a 120-mesh square-hole sieve to obtain a first oversize product and a first undersize product.
4. The method of claim 1, wherein the specific operation of the step 3) of attracting the magnetic wrap with a magnet to the first oversize material is: and (4) sucking the magnetic wrappage on the first oversize product by using a paper wrapped magnet until the magnetic wrappage is completely sucked.
5. The method of claim 1, wherein the second oversize material in step 4) is reground, crushed and sieved using an internal pulverizer, and then all is sieved through a 120-mesh square-hole sieve.
6. The method according to claim 1, wherein the specific steps of determining the content of TFe in the first test sample and the second test sample respectively by using the chemical analysis method in step 5) are as follows:
6.1, quantitatively weighing a sample in a 300mL triangular flask, adding 20mL sulfuric acid-phosphoric acid mixed acid, dissolving the mixture on a high-temperature electric furnace until sulfuric acid fume leaves the bottom of the flask to the height of one half of the flask, taking down the flask for slight cooling, adding 20mL hydrochloric acid (1+1), reducing the mixture to light yellow by using a 60g/L tin dichloride solution, taking down the flask for slight cooling, and adding 50mL hot water to keep the temperature of the solution at 40-50 ℃;
6.2, adding 8 drops of sodium tungstate solution with the concentration of 250g/L, reducing the solution to stable blue by using titanium trichloride solution (1+9), dripping potassium dichromate standard solution with the concentration of 0.05mol/L until the blue disappears, immediately adding four drops of diphenylamine sodium sulfonate solution with the concentration of 4g/L, titrating the potassium dichromate standard solution with the concentration of 0.05mol/L to stable purple as an end point, recording the volume (mL) of the titration, synchronously adopting a blank reagent as a control, and calculating the content of TFe in the sample by using the following formula:
in the formula:
V0: volume of potassium dichromate standard titration solution (mL) consumed for blank reagents;
v: volume (mL) of potassium dichromate standard titration solution consumed by the sample;
c: concentration (mol/L) of potassium dichromate standard titration solution;
m: sample mass (g);
m: molar mass of iron (55.85 g/mol);
wherein the TFe content in the obtained first test sample is W (TFe)1) (%), the TFe content in the second test sample was W (TFe)2)(％)。
7. The method according to claim 6, wherein the sulfuric acid-phosphoric acid mixed acid in step 6.1 is prepared by: slowly injecting 150mL of sulfuric acid with the concentration of 1.84g/mL into 700mL of water under stirring, cooling, then adding 150mL of phosphoric acid with the concentration of 1.70g/mL, and uniformly mixing;
the preparation method of the titanium trichloride solution in the step 6.2 comprises the following steps: 1 part of titanium trichloride solution with the mass concentration of 15-20% is transferred and added with 9 parts of hydrochloric acid (1+3) to be mixed evenly.
8. The method according to claim 6 or 7, wherein the formula for calculating the TFe content in the steel slag magnetic separation powder in the step 6) is as follows:
W(TFe)(％)＝(m1×W(TFe1)(％)+m2×W(TFe2)(％))/m0
wherein:
m0the mass (g) of a sample to be detected;
m1is the first test sample mass (g), i.e., m0-m2；
m2Is the second test sample mass (g);
W(TFe1) (%) represents the content of TFe in the first test sample;
W(TFe2) (%) represents the content of TFe in the second test sample;
w (tfe) (%): and (4) determining the TFe content in the sample to be tested.
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| CN112414887A (en) * | 2020-10-30 | 2021-02-26 | 攀枝花钢城集团有限公司 | Method for measuring content of metallic iron in medium-low grade slag steel iron |
| CN113466079A (en) * | 2021-06-30 | 2021-10-01 | 重庆钢铁股份有限公司 | Method for detecting component content of steel slag |
| CN113466079B (en) * | 2021-06-30 | 2023-05-16 | 重庆钢铁股份有限公司 | Method for detecting content of steel slag components |
| CN115015469A (en) * | 2022-06-28 | 2022-09-06 | 酒泉钢铁(集团)有限责任公司 | Method for detecting total iron content of steel slag |
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