CN103604687B - A kind of method utilizing electrolysis magnetic method complete extraction steel inclusion - Google Patents
A kind of method utilizing electrolysis magnetic method complete extraction steel inclusion Download PDFInfo
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- CN103604687B CN103604687B CN201310647043.4A CN201310647043A CN103604687B CN 103604687 B CN103604687 B CN 103604687B CN 201310647043 A CN201310647043 A CN 201310647043A CN 103604687 B CN103604687 B CN 103604687B
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Abstract
The invention discloses a kind of method utilizing electrolysis magnetic method complete extraction steel inclusion, belong to metal physics research method technical field.Step of the present invention is: (1) prepares steel sample; (2) electrolytic process, using steel sample as anode, and puts into electrolytic tank by steel sample and carries out electrolysis; (3) eluriate process, control the gas velocity of draft tube and the water velocity of water inlet pipe; (4) magnetic separation is separated, and magnetic separation is separated ware and is fixed on Vib., and electromagnet is installed in the top that magnetic separation is separated ware, does is the vibration frequency controlling Vib. 1 ~ 5? Hz, does is horizontal vibration amplitude 2 ~ 4? cm, while magnetic separation separation ware is with Vib. vibration, is separated iron powder magnetic separation by electromagnet; (5) snotter classification and weighing.The present invention effectively can stop the adsorpting aggregation of iron powder and snotter, because suction-operated encasing inclusion when preventing iron powder to be separated by magnetic separation, thus avoids the loss of snotter, substantially increases the accuracy that snotter measures.
Description
Technical field
The present invention relates to metal physics research method technical field, more particularly, relate to a kind of method utilizing electrolysis magnetic method complete extraction steel inclusion.
Background technology
The performance of steel depends on the composition of steel inclusion, pattern, size and distributed number to a certain extent.And steel inclusion is usually in diversity, the size of inclusion particle differs, and large particle diameter may more than 20 μm, and little particle diameter may at below 50nm, and the chemical composition of different size snotter is also inconsistent.The snotter that these grain sizes, chemical composition differ role in different steel is different.In order to comprehensively deep research snotter is on the impact of iron and steel performance, needs to extract intact for these snotteres not of uniform size from steel, and by scanning electron microscope, accurate analysis is carried out to its composition, pattern, size and distributed number.
At present, generally microscopic method is had to the method for inclusion analysis, electrolysis of small sample method or bulk sample electrolysis method etc., the basic experiment step of bulk sample electrolysis method is existing similar open in the prior art, as China Patent No. 201210276465.0, the applying date is on August 3rd, 2012, invention and created name is: a kind of method utilizing electrolytic process to measure the medium-and-large-sized non-metallic inclusion of steel, the step of this application case is as follows: (1), electrolysis prepares: require specimen finish 30 ~ 50mm, height is 140 ~ 180mm, center, sample one end is drilled with screw, sample weight 2 ~ 5Kg, negative electrode is entanglement, electrolytic solution consists of 6 ~ 15%FeCl
2, 2 ~ 4%FeSO
4, 5 ~ 8%ZnCl
2, 0.2 ~ 0.5% citric acid, all the other are distilled water, (2), electrolysis: sample connects on the line by serial arrangement, and each sample is about 2 ~ 5V voltage drop, and electrolysis time is 7 ~ 10 days, (3), eluriate: earth of positive pole liquid 100 ~ 200ml is poured into and eluriates in groove, first open N
2stir, N
2airshed controls at 0.5 ~ 0.8L/min, and the elutriation time is 20-30 minute, (4), reduce: logical N
2oxygen in cleaning air-channel system, and make diamond heating 0.5 ~ 1.0 hour, cut off N
2, change logical H
2, logical H
2furnace temperature keeps 350 ~ 500 DEG C and cuts off the electricity supply for about 2 hours, allows electric furnace at logical H
2be cooled to temperature in situation lower than 200 DEG C, glass boat to be taken out, then carry out magnetic separation and select iron and ferromagnetic oxide, (5), snotter classification and weighing: use standard small bolter, sieve and calculate percentage composition at different levels.
But, there is following difficulty to the detachment process of snotter in the bulk sample electrolysis method of prior art: (1) snotter easily loses in leaching process, especially in the reduction also magnetic separation stage, because electrolysis and reduction after iron powder and inclusion size all very tiny, specific surface energy is larger, iron powder and snotter is made very easily to reunite and be attached together, when magnetic separation is carried out to the potpourri of iron powder and snotter, snotter is wrapped in by iron powder, be easy to a snotter while being separated iron powder also separate, the content of snotter is caused to lose in a large number, have a strong impact on the accuracy of test findings, in order to prevent snotter when magnetic separation by adsorptive separation, a large amount of iron powders is retained in magnetic separation process of being everlasting, then the iron powder after magnetic separation is placed and sort snotter under the microscope, sort the work extremely time and effort consuming of snotter under the microscope, and very likely cause snotter to be retained in iron powder, test findings is caused to depart from real data, thus the accurate analysis of impact test.(2) in high temperature reduction process, part snotter may decompose, and changes the composition of snotter, is unfavorable for the accurate analysis to snotter.Bulk sample electrolysis method complex steps of the prior art, each step all can have the loss of snotter, cannot accomplish to extract intact for snotter from steel.
Summary of the invention
1. invent the technical matters that will solve
When the object of the invention is to overcome bulk sample electrolysis method in prior art there is following technical matters in snotter isolation technics: (1), part snotter are easily etched or easily lose in collection process in leaching process, are difficult to accomplish to collect without loss; (2), when carrying out magnetic separation to snotter and being separated, because snotter and the iron powder extracted easily adsorbs reunion usually, very difficult snotter to be extracted completely from iron powder.The invention provides a kind of method utilizing electrolysis magnetic method complete extraction steel inclusion, adopt technical scheme of the present invention, snotter almost can be extracted in intact lost territory from steel, substantially increase the accuracy that snotter measures.
2. technical scheme
For achieving the above object, technical scheme provided by the invention is:
A kind of method utilizing electrolysis magnetic method complete extraction steel inclusion of the present invention, the steps include:
Step one, prepare steel sample
Get steel sample from steel billet to be analyzed, described steel sample is rectangular structure, and it is long is 8cm, and wide is 6cm, is highly 10cm, removes the surface oxide layer of steel sample, and polishes to steel sample surface;
Step 2, electrolytic process
Using the steel sample of step one as anode, and steel sample is put into electrolytic tank carry out electrolysis, its electrolytic solution is: 1% citric acid, 1% sodium citrate, 3% zinc chloride, 5% green vitriol, 0.5% ascorbic acid and distilled water, 10 ~ 50mL triglyceride covers the upper surface of electrolytic solution, Current Control is 6.0A, when electrolysis starts, pH value controls is 6.0, every 12 hours, the pH value of electrolytic solution is measured with pH test paper, when electrolytic solution pH value lower than 6.0 time, by dripping citric acid, to control the pH value of electrolytic solution be 6.0; Electrolysis time is 96 hours, electrolysis temperature controls at 0 DEG C, electrolytic process terminates rear taking-up anode steel sample, and it is surperficial with distilled water flushing anode steel sample, the electrolyte on steel sample surface is rinsed well and entered electrolytic tank, by the earth of positive pole in electrolytic tank and solution left standstill 24 hours, after leaving standstill when ensureing that the earth of positive pole is static, upper solution is removed;
Step 3, elutriation process
Earth of positive pole step 2 obtained and surplus solution are transferred in the elutriation groove body of washing device, first feed opening is sealed before transfer, wire netting is positioned in washing trough body after transfer, wire netting is fixed on washing trough body by interior metal support, and adjust the water velocity of water inlet pipe and the gas velocity of draft tube, wherein: the gas velocity of draft tube requires bottom port outflow per second 0.5 ~ 1 bubble of draft tube, argon gas is passed in draft tube, the water velocity of water inlet pipe is 0.2L/min, distilled water is passed in water inlet pipe, carry out elutriation process afterwards, the elutriation time is 24 hours, after elutriation terminates, close the valve of draft tube and draft tube, and remove wire netting and interior metal support, again leave standstill 24 hours, discharged by supernatant in washing trough body after leaving standstill, the remaining earth of positive pole and distilled water move to magnetic separation from feed opening and are separated ware, wherein: described washing device comprises support, eluriates groove body, interior metal support, wire netting, water inlet pipe, rising pipe, draft tube, gas outlet and feed opening, described elutriation groove body is divided into upper and lower, and its top is cylindrical structure, and its underpart is conical structure, and this elutriation groove body is fixed on support, described elutriation groove body is provided with draft tube and gas outlet, and the bottom of this draft tube extends to the bottom of eluriating groove body, and this gas outlet is positioned at the top of eluriating groove body, described elutriation groove body is provided with water inlet pipe and rising pipe, and this rising pipe is positioned on the sidewall of elutriation groove bodies top, described wire netting is fixed on by interior metal support eluriates groove body interior,
Step 4, magnetic separation are separated
The magnetic separation that the earth of positive pole and distilled water are housed in step 3 is separated ware is fixed on Vib., and above magnetic separation separation ware, electromagnet is installed, the inner bottom surface of described magnetic separation separation ware is distributed with isolation pin, this isolation pin is the Rotary-table structure vertically arranged, its base diameter is 2mm, upper diameter is 1mm, is highly 5mm, and the distance between isolation pin is adjacent is 2 ~ 4mm; The vibration frequency controlling Vib. is 1 ~ 5Hz, and horizontal vibration amplitude is 2 ~ 4cm, while magnetic separation separation ware is with Vib. vibration, iron powder magnetic separation is separated by electromagnet;
Step 5, snotter classification and weigh
The earth of positive pole after step 5 magnetic separation being separated is dry under the atmosphere of argon shield; standard bolter is used after dry; sieve as being greater than 60 μm, 50 ~ 60 μm, 40 ~ 50 μm, 20 ~ 40 μm, be less than 20 μm of Pyatyis altogether, classification is weighed weight at different levels, and calculates percentage composition at different levels.
Preferably, in step 4 magnetic separation detachment process, the distance between magnetic separation separation ware interior isolation pin is adjacent is 3mm, and the vibration frequency of Vib. is 3Hz, and horizontal vibration amplitude is 3cm.
3. beneficial effect
Adopt technical scheme provided by the invention, compared with existing known technology, there is following remarkable result:
A kind of method utilizing electrolysis magnetic method complete extraction steel inclusion of the present invention, magnetic separation is separated the inner a large amount of isolation pin of ware and the earth of positive pole can be made to be dispersed in different area of space, stop the adsorpting aggregation of iron powder and snotter, thus because suction-operated encasing inclusion when can effectively prevent iron powder to be separated by magnetic separation, thus avoid the loss of snotter, ensure that the Accurate Measurement of snotter; Meanwhile, in the present invention, vibration frequency and the amplitude of Vib. can ensure that the distilled water that magnetic separation is separated ware inside is in certain turbulence state, can snotter be made further to be separated with iron powder.Isolation pin and Vib. acting in conjunction; play the coordinative role of multiple protective, prevent snotter to be wrapped in iron powder, reach good snotter separating effect through site test; solve steel inclusion and be difficult to the intact difficult problem losing extraction, substantially increase the accuracy that snotter measures.This invention simplifies the flow process that steel inclusion extracts, not only can remove heat reduction process from, sort the tedious work of snotter under even can removing Electronic Speculum from, substantially increase work efficiency and accuracy rate.
Accompanying drawing explanation
Fig. 1 is the structural representation of washing device in the present invention;
Fig. 2 is the schematic diagram that in the present invention, magnetic separation is separated;
Fig. 3 is the structural representation that in the present invention, magnetic separation is separated ware.
Label declaration in schematic diagram: 1, support; 2, groove body is eluriated; 31, interior metal support; 32, wire netting; 41, water inlet pipe; 42, rising pipe; 51, draft tube; 52, gas outlet; 6, feed opening; 7, magnetic separation is separated ware; 701, pin is isolated; 8, Vib.; 9, electromagnet.
Embodiment
For understanding content of the present invention further, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.
embodiment 1
A kind of method utilizing electrolysis magnetic method complete extraction steel inclusion of the present embodiment, its concrete steps are as follows:
Step one, prepare steel sample
Get steel sample from steel billet to be analyzed, described steel sample is rectangular structure, and it is long is 8cm, and wide is 6cm, is highly 10cm, and the quality of steel sample is 3.768kg, removes the surface oxide layer of steel sample, and polishes to steel sample surface.
Step 2, electrolytic process
Using the steel sample of step one as anode, and steel sample is put into electrolytic tank carry out electrolysis, its electrolytic solution is: 1%(mass percent) citric acid, 1%(mass percent) sodium citrate, 3%(mass percent) zinc chloride, 5%(mass percent) green vitriol, 0.5%(mass percent) ascorbic acid and distilled water, wherein: citric acid, as buffering agent, prevents the pH value big ups and downs of electrolytic solution; Sodium citrate, as sequestrant, makes the oxide of sodium citrate and iron react the complex compound produced and can be good at dissolving; ZnCl
2as resistance to blunt agent, prevent from producing passivating film during electrolysis, affect current density, increase electrolysis time; Ascorbic acid as reductive agent, anti-oxidation.30mL triglyceride covers the upper surface of electrolytic solution, and the object adding triglyceride is isolated air, prevents electrolysis anode sludge to be oxidized.Current Control is 6.0A, and when electrolysis starts, pH value controls to be 6.0 every 12 hours, measures the pH value of electrolytic solution with pH test paper, when electrolytic solution pH value lower than 6.0 time, the pH value controlling electrolytic solution by dripping citric acid is 6.0; Electrolysis time is 96 hours, electrolysis temperature controls at 0 DEG C, electrolytic process terminates rear taking-up anode steel sample, and it is surperficial with distilled water flushing anode steel sample, the electrolyte on steel sample surface is rinsed well and entered electrolytic tank, by the earth of positive pole in electrolytic tank and solution left standstill 24 hours, after leaving standstill when ensureing that the earth of positive pole is static, upper solution is removed; The present embodiment is by the electrolytic solution of customized configuration, and the pH value keeping electrolytic solution is particular value, and electrolytic process is fully carried out, and guarantees that all types of steel inclusion all enters the earth of positive pole.
Step 3, elutriation process
In order to remove remaining electrolytic solution residual fraction in the earth of positive pole, antianode mud is needed to eluriate.Earth of positive pole step 2 obtained and surplus solution are transferred in the elutriation groove body 2 of washing device, first feed opening 6 is sealed before transfer, after transfer, wire netting 32 is positioned in washing trough body 2, wire netting 32 is fixed on washing trough body 2 by interior metal support 31, and adjust the water velocity of water inlet pipe 41 and the gas velocity of draft tube 51, wherein: the gas velocity of draft tube 51 requires bottom port outflow per second 0.5 ~ 1 bubble of draft tube 51, bottom port outflow per second 1 bubble of draft tube 51 is controlled in the present embodiment, argon gas is passed in draft tube 51, the water velocity of water inlet pipe 41 is 0.2L/min, distilled water is passed in water inlet pipe 41, carry out elutriation process afterwards, the elutriation time is 24 hours.By controlling the gas velocity of draft tube 51 and the water velocity of water inlet pipe 41, the water droplet of rising pipe 42 is made to be cotton-shaped outflow, and coordinate the gas velocity of draft tube 51, guarantee that the earth of positive pole is obtaining under the condition fully eluriated, snotter almost in the complete reservation earth of positive pole, in order to avoid air-flow or current excessive, the earth of positive pole is gone out and eluriates groove body 2.After elutriation terminates, close the valve of draft tube 51 and draft tube 51, and remove wire netting 32 and interior metal support 31, again leave standstill 24 hours, discharged by supernatant in washing trough body 2 after leaving standstill, the remaining earth of positive pole and distilled water move to magnetic separation from feed opening 6 and are separated ware 7.
As shown in Figure 1, the washing device in the present embodiment comprises support 1, eluriates groove body 2, interior metal support 31, wire netting 32, water inlet pipe 41, rising pipe 42, draft tube 51, gas outlet 52 and feed opening 6; Described elutriation groove body 2 is divided into upper and lower, and its top is cylindrical structure, and its underpart is conical structure, and this elutriation groove body 2 is fixed on support 1; Described elutriation groove body 2 is provided with draft tube 51 and gas outlet 52, and the bottom of this draft tube 51 extends to the bottom of eluriating groove body 2, and this gas outlet 52 is positioned at the top of eluriating groove body 2; Described elutriation groove body 2 is provided with water inlet pipe 41 and rising pipe 42, and this rising pipe 42 is positioned on the sidewall at elutriation groove body 2 top; Described wire netting 32 is fixed on by interior metal support 31 eluriates groove body 2 inside.Adopt bottom to be that conical structure eluriates groove body 2 in the present embodiment, conveniently the earth of positive pole is moved to magnetic separation from feed opening 6 and be separated ware 7, and the transfer completely of the earth of positive pole can be ensured, thus ensure the complete collection of snotter.
Step 4, magnetic separation are separated
The magnetic separation that the earth of positive pole and distilled water are housed in step 3 is separated ware 7 is fixed on Vib. 8, and above magnetic separation separation ware 7, electromagnet 9 is installed, the inner bottom surface of described magnetic separation separation ware 7 is distributed with isolation pin 701(as shown in Figure 3), this isolation pin 701 is the Rotary-table structure vertically arranged, its base diameter is 2mm, upper diameter is 1mm, is highly 5mm, and the distance between isolation pin 701 is adjacent is 3mm; The vibration frequency controlling Vib. 8 is 3Hz, horizontal vibration amplitude is 3cm, while magnetic separation separation ware 7 vibrates with Vib. 8, by electromagnet 9, iron powder magnetic separation is separated, electromagnet 9 in the present embodiment adopts ring electromagnet, the magnetic of electromagnet 9 can be changed by changing coil current in real time, reaching optimum condition to make the magnetic separation separating effect of iron powder.
As one of outstanding improvement of the present invention, magnetic separation is separated the inner a large amount of isolation pin 701 of ware 7 and the earth of positive pole can be made to be dispersed in different area of space, stop the adsorpting aggregation of iron powder and snotter, thus because suction-operated encasing inclusion when can effectively prevent iron powder to be separated by magnetic separation, thus avoid the loss of snotter, ensure that the Accurate Measurement of snotter.Meanwhile, in the present embodiment, vibration frequency and the amplitude of Vib. 8 can ensure that the distilled water that magnetic separation is separated ware 7 inside is in certain turbulence state, can snotter be made further to be separated with iron powder.Above-mentioned isolation pin 701 and Vib. 8 acting in conjunction, play the coordinative role of multiple protective, prevents snotter to be wrapped in iron powder, reaches good snotter separating effect through site test.
In addition, it is all undertaken being in air after earth of positive pole elutriation, drying, reduction that magnetic separation of the prior art is separated, the adsorpting aggregation problem of its snotter and iron powder is difficult to solve always, the earth of positive pole is positioned in distilled water by the present invention, and by electromagnet 9, iron powder magnetic separation is separated, the separating effect of the discovery iron powder that applicant is surprised and snotter is very remarkable, does not almost adsorb agglomeration traits between snotter and iron powder.The present invention, in order to improve the absorption reunion situation between snotter and iron powder further, promotes the separation between snotter and iron powder, and oxidation of iron powder when preventing magnetic separation, can be separated in ware 7 in magnetic separation and add the ascorbic acid that mass percent is 1%.In the present invention, the schematic diagram of magnetic separation separation as shown in Figure 2, wherein: iron powder stressing conditions when liquid gas interface is as follows: F
1for electromagnetic force, F
2for surface tension, G is the gravity (because the volume of iron powder is little, buoyancy is not considered) of iron powder.Iron powder penetrates liquid-gas interface under the action of a magnetic force, and uniform adsorption, on electromagnet 9, reaches the object being separated iron powder and steel inclusion.Iron powder will overcome the gravity of iron powder and the resistance of water under liquid level, when penetrating liquid gas interface, not only will overcome the gravity of iron powder, also will overcome the surface tension of liquid gas interface layer to iron powder.Thermodynamic definitions from soaking: after solid and liquid comes into contact, the whole system free enthalpy of solid and liquid reduces, specific surface energy reduces, absorption affinity between iron powder and snotter is weakened, when the faint absorption affinity existed is less than the surface tension of liquid to snotter, again because the effect of electromagnetic force, be separated so iron powder can penetrate liquid level by magnetic separation, but snotter can not stay in a liquid by electromagnetic force upwards, thus reach snotter and be separated with the thorough of iron powder.The technical scheme of the present embodiment can under the not removed condition of guarantee snotter, maximum separation iron powder, decrease the sorting work amount under Electronic Speculum, even do not need Electronic Speculum process just can meet the requirement of experiment, and the small-sized snotter of less than 50 μm can be obtained.
Step 5, snotter classification and weigh
The earth of positive pole after step 5 magnetic separation being separated is dry under the atmosphere of argon shield; standard bolter is used after dry; sieve as being greater than 60 μm, 50 ~ 60 μm, 40 ~ 50 μm, 20 ~ 40 μm, be less than 20 μm of Pyatyis altogether, classification is weighed weight at different levels, and calculates percentage composition at different levels.
embodiment 2
A kind of method utilizing electrolysis magnetic method complete extraction steel inclusion of the present embodiment, its basic step is with embodiment 1, difference is: in step 4 magnetic separation detachment process, distance between the interior isolation pin 701 of magnetic separation separation ware 7 is adjacent is 2mm, the vibration frequency of Vib. 8 is 5Hz, and horizontal vibration amplitude is 4cm.
embodiment 3
A kind of method utilizing electrolysis magnetic method complete extraction steel inclusion of the present embodiment, its basic step is with embodiment 1, difference is: in step 4 magnetic separation detachment process, distance between the interior isolation pin 701 of magnetic separation separation ware 7 is adjacent is 4mm, the vibration frequency of Vib. 8 is 1Hz, and horizontal vibration amplitude is 2cm.
A kind of method utilizing electrolysis magnetic method complete extraction steel inclusion of embodiment 1 ~ 3, magnetic separation is separated the inner a large amount of isolation pin 701 of ware 7 and the earth of positive pole can be made to be dispersed in different area of space, stop the adsorpting aggregation of iron powder and snotter, thus because suction-operated encasing inclusion when can effectively prevent iron powder to be separated by magnetic separation, thus avoid the loss of snotter, ensure that the Accurate Measurement of snotter, substantially increase the accuracy that snotter measures.
Claims (2)
1. utilize a method for electrolysis magnetic method complete extraction steel inclusion, it is characterized in that, the steps include:
Step one, prepare steel sample
Get steel sample from steel billet to be analyzed, described steel sample is rectangular structure, and it is long is 8cm, and wide is 6cm, is highly 10cm, removes the surface oxide layer of steel sample, and polishes to steel sample surface;
Step 2, electrolytic process
Using the steel sample of step one as anode, and steel sample is put into electrolytic tank carry out electrolysis, its electrolytic solution is: 1% citric acid, 1% sodium citrate, 3% zinc chloride, 5% green vitriol, 0.5% ascorbic acid and distilled water, 10 ~ 50mL triglyceride covers the upper surface of electrolytic solution, Current Control is 6.0A, when electrolysis starts, pH value controls is 6.0, every 12 hours, the pH value of electrolytic solution is measured with pH test paper, when electrolytic solution pH value lower than 6.0 time, by dripping citric acid, to control the pH value of electrolytic solution be 6.0; Electrolysis time is 96 hours, electrolysis temperature controls at 0 DEG C, electrolytic process terminates rear taking-up anode steel sample, and it is surperficial with distilled water flushing anode steel sample, the electrolyte on steel sample surface is rinsed well and entered electrolytic tank, by the earth of positive pole in electrolytic tank and solution left standstill 24 hours, after leaving standstill when ensureing that the earth of positive pole is static, upper solution is removed;
Step 3, elutriation process
Earth of positive pole step 2 obtained and surplus solution are transferred in the elutriation groove body (2) of washing device, first feed opening (6) is sealed before transfer, after transfer, wire netting (32) is positioned in washing trough body (2), wire netting (32) is fixed on washing trough body (2) by interior metal support (31), and adjust the water velocity of water inlet pipe (41) and the gas velocity of draft tube (51), wherein: the gas velocity of draft tube (51) requires bottom port outflow per second 0.5 ~ 1 bubble of draft tube (51), draft tube passes into argon gas in (51), the water velocity of water inlet pipe (41) is 0.2L/min, water inlet pipe passes into distilled water in (41), carry out elutriation process afterwards, the elutriation time is 24 hours, after elutriation terminates, close the valve of draft tube (51) and draft tube (51), and remove wire netting (32) and interior metal support (31), again leave standstill 24 hours, discharged by interior for washing trough body (2) supernatant after leaving standstill, the remaining earth of positive pole and distilled water move to magnetic separation from feed opening (6) and are separated ware (7),
Wherein: described washing device comprises support (1), eluriates groove body (2), interior metal support (31), wire netting (32), water inlet pipe (41), rising pipe (42), draft tube (51), gas outlet (52) and feed opening (6); Described elutriation groove body (2) is divided into upper and lower, and its top is cylindrical structure, and its underpart is conical structure, and this elutriation groove body (2) is fixed on support (1); Described elutriation groove body (2) is provided with draft tube (51) and gas outlet (52), the bottom of this draft tube (51) extends to the bottom of eluriating groove body (2), and this gas outlet (52) is positioned at the top of eluriating groove body (2); Described elutriation groove body (2) is provided with water inlet pipe (41) and rising pipe (42), this rising pipe (42) is positioned on the sidewall at elutriation groove body (2) top; Described wire netting (32) is fixed on by interior metal support (31) eluriates groove body (2) inside;
Step 4, magnetic separation are separated
The magnetic separation that the earth of positive pole and distilled water are housed in step 3 is separated ware (7) is fixed on Vib. (8), and top installation electromagnet (9) of ware (7) is separated in magnetic separation, the inner bottom surface of described magnetic separation separation ware (7) is distributed with isolation pin (701), this isolation pin (701) is the Rotary-table structure vertically arranged, its base diameter is 2mm, upper diameter is 1mm, be highly 5mm, the distance between isolation pin (701) is adjacent is 2 ~ 4mm; The vibration frequency controlling Vib. (8) is 1 ~ 5Hz, and horizontal vibration amplitude is 2 ~ 4cm, while magnetic separation separation ware (7) is vibrated with Vib. (8), iron powder magnetic separation is separated by electromagnet (9);
Step 5, snotter classification and weigh
The earth of positive pole after step 4 magnetic separation being separated is dry under the atmosphere of argon shield; standard bolter is used after dry; sieve as being greater than 60 μm, 50 ~ 60 μm, 40 ~ 50 μm, 20 ~ 40 μm, be less than 20 μm of Pyatyis altogether, classification is weighed weight at different levels, and calculates percentage composition at different levels.
2. a kind of method utilizing electrolysis magnetic method complete extraction steel inclusion according to claim 1, it is characterized in that: in step 4 magnetic separation detachment process, distance between magnetic separation separation ware (7) interior isolation pin (701) is adjacent is 3mm, the vibration frequency of Vib. (8) is 3Hz, and horizontal vibration amplitude is 3cm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2559984Y (en) * | 2002-07-25 | 2003-07-09 | 宝钢集团上海梅山有限公司 | Datail electrolytic equipment |
| CN201001992Y (en) * | 2007-01-18 | 2008-01-09 | 宝钢集团上海梅山有限公司 | Bulk sample electrolysis equipment elutriation trough |
| CN102778377A (en) * | 2012-08-03 | 2012-11-14 | 北京科技大学 | Electrolysis determination method of macro nonmetallic inclusions in steel |
| CN102818723A (en) * | 2012-09-07 | 2012-12-12 | 首钢总公司 | Method of electrolytically extracting and detecting fine inclusions in steel |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3489015B2 (en) * | 1995-08-31 | 2004-01-19 | 株式会社ホタニ | Strip cleaning wastewater treatment method and apparatus, and magnetic separator |
-
2013
- 2013-12-06 CN CN201310647043.4A patent/CN103604687B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2559984Y (en) * | 2002-07-25 | 2003-07-09 | 宝钢集团上海梅山有限公司 | Datail electrolytic equipment |
| CN201001992Y (en) * | 2007-01-18 | 2008-01-09 | 宝钢集团上海梅山有限公司 | Bulk sample electrolysis equipment elutriation trough |
| CN102778377A (en) * | 2012-08-03 | 2012-11-14 | 北京科技大学 | Electrolysis determination method of macro nonmetallic inclusions in steel |
| CN102818723A (en) * | 2012-09-07 | 2012-12-12 | 首钢总公司 | Method of electrolytically extracting and detecting fine inclusions in steel |
Non-Patent Citations (2)
| Title |
|---|
| 水溶液电解法提取钢种超细非金属夹杂物研究;李慧改 等;《上海金属》;20101130;第32卷(第6期);39-42,46 * |
| 钢中大型夹杂物的提取与分离;孙辰龄;《北京科技大学学报》;19940831;第16卷(第4期);392-395 * |
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