CN101844753A - Method for recovering phosphorus element from converter duplex dephosphorized slag - Google Patents

Method for recovering phosphorus element from converter duplex dephosphorized slag Download PDF

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CN101844753A
CN101844753A CN 201010171945 CN201010171945A CN101844753A CN 101844753 A CN101844753 A CN 101844753A CN 201010171945 CN201010171945 CN 201010171945 CN 201010171945 A CN201010171945 A CN 201010171945A CN 101844753 A CN101844753 A CN 101844753A
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slag
phosphorus
dephosphorized slag
converter
phosphoric
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CN101844753B (en
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刁江
谢兵
王永红
王雨
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Chongqing University
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Abstract

The invention discloses a method for recovering a phosphorus element from converter duplex dephosphorized slag, which comprises the following steps of: changing a phase composition and distribution of elements of the dephosphorized slag by adding acid or neutral oxides SiO2, Al2O3 and TiO2 so as to allow the phosphorus element in the slag to enrich in a phosphorus-rich phase; controlling the total content of SiO2, Al2O3 and TiO2 in a mixture of the dephosphorized slag and a modifier to account for 25 to 40 percent of the total weight; performing high-temperature melting treatment on the mixture; controlling the initial cooling temperature of the slag to be over 1,500 DEG C, wherein a cooling rate of a temperature interval over 1, 200 DEG C is less than or equal to 10 DEG C/minute; and crushing the condensed slag to below 20mm, and performing fine grinding on the slag to below 30 meshes in a ball mill. A phosphorus-rich nonmagnetic substance is separated from a low-phosphorus magnetic substance by a magnetic separation method, and the recovered phosphorus-rich phase can be used as a raw material of an agricultural phosphorus fertilizer. A low-phosphorus phase which is rich in an iron element, a manganese element and the like can return to a converter to be used, so that the aims of saving the energy, reducing the emission and reducing the steel production cost are fulfilled.

Description

The recovery method of phosphoric in the converter duplex dephosphorized slag
Technical field
The present invention relates to the method that a kind of metallurgical slag resource utilization is utilized again, be specifically related to a kind of treatment process that from converter duplex smelting technology dephosphorization stove slag, reclaims phosphoric.
Background technology
Converter slag is the byproduct of steelmaking process, is one of main solid waste of iron and steel metallurgical industry.At present, the Iron and Steel Enterprises in China converter quantity of slag is generally 10～15% of crude steel output.Chinese crude steel output was 5.68 hundred million tons in 2009, and the converter steel ratio is about 88%.The annual converter slag byproduct that brings thus is up to 5000～7,500 ten thousand tons.Compared with developed countries, China's converter slag comprehensive utilization ratio is lower, only is 36% at present, simultaneously, utilizes level relatively backward, is generally used for producing cement, engineering backfill, makes steel slag brick and returns sintering etc.Belong to elementary utilization under the situation mostly, fail to give full play to the resource value of converter slag.Remain a large amount of waste residues and still stack processing, take the good farmland, contaminate environment influences the Sustainable development of people and society.
The converter duplex method is a kind of ultra-low phosphoretic steel smelting technology of rising in recent years.This technology is at first carried out dephosphorization treatment to molten iron in a special-purpose converter, decarburization steel-making is carried out in another converter of packing into of the molten iron behind the dephosphorization.Adopt special-purpose converter, the favourable condition that can make full use of interior oxidizing atmosphere of stove and strong bottom blowing stirring is carried out dephosphorization, can realize few slag blowing during steel-making.P in the decarburization stove slag 2O 5Low with S content, can return the dephosphorization stove and use.Owing to adopt special-purpose converter dephosphorization, the P in the dephosphorization stove slag 2O 5Content often is higher than conventional converter slag, it is returned sintering and iron manufacturing process certainly will cause the molten iron phosphorus content to improve constantly, and increases the steel making working procedure burden; So dephosphorization stove slag generally can't melt down utilization again, must discharge the back otherwise processed, utilize again after can be used for making brick.Dephosphorization stove terminal temperature far below conventional smelting converter tapping temperature, thereby free oxidation calcium contents height in the dephosphorized slag, is used it for building field and need be handled through secular ageing usually about 1350 ℃.In view of the higher relatively P of dephosphorized slag 2O 5Content, it is excellent thomas phosphate raw material.Especially during high phosphorus hot metal, can obtain high P during converter duplex is smelted 2O 5The dephosphorized slag of content can obtain high-quality thomas phosphate to its further processing, promotes the recycling of bessemer furnace slag at agriculture field, solves environmental pollution and creates economic benefit.
For realizing the recycling of converter slag at agriculture field, the metallargist has developed the enrichment and the isolation technique of multiple phosphorus, comprises utilizing density variation slow cooling come-up, reduction separation, electrolytic separation, flotation separation etc.Because conventional converter slag P 2O 5Some defectives that lower and above-mentioned each method self of content exists still do not have effective means at present and obtain practical application in industry.Converter duplex technology and conventional single converter smelting process are very different: at first dephosphorization stove terminal temperature is usually about 1350 ℃, than low about 300 ℃ of conventional converter tapping temperature; Next dephosphorization stove smelting cycle instrument 8～12min is far below single converter smelting.The difference of processing parameter makes dephosphorized slag and conventional converter slag be very different on microstructure.Because system temperature is low, the time is short, mineral in the dephosphorized slag are difficult to as the abundant gathering growth of conventional converter slag, cause rich phosphorus thing phase size much smaller than grinding fineness, and phosphorus, iron disperse distribute, rich phosphorus phase and rich iron phase embedding cloth are tight, adopt traditional separating technology to be difficult to effectively the phosphoric in the dephosphorized slag be recycled.
Summary of the invention
A difficult problem that is difficult to effectively separate phosphoric in the converter duplex dephosphorized slag at above-mentioned traditional separating technology, the objective of the invention is to: a kind of method of effectively separating and reclaim phosphoric from converter duplex dephosphorized slag is provided, and the rich phosphorus after the separation can be used for agriculture field mutually; Another object of the present invention is to, when separating phosphoric, reclaim the low-phosphorous phase that is rich in elements such as iron, manganese, it is returned converter use, thereby realize energy-saving and emission-reduction, reduction STEELMAKING PRODUCTION cost.
For achieving the above object, the present invention has adopted following technical scheme:
The recovery method of phosphoric in the converter duplex dephosphorized slag, its characteristics are: add acidity or neutral oxide as properties-correcting agent in dephosphorized slag; The mixture of dephosphorized slag and properties-correcting agent is carried out high-temperature fusion handle, make properties-correcting agent change dephosphorized slag thing phase composite and element distributes, make phosphoric in the slag be enriched in one or the one group of stable mineral; To the mixture cooling after the above-mentioned high-temperature fusion processing, cooled mixture slag specimen carries out magnetic separation behind fragmentation, ball milling separates, and obtains the nonmagnetics of rich phosphorus and low-phosphorous magnetic thing.
The applicant analyzes, and the phosphorus in the dephosphorized slag is mainly with 3CaOP 2O 5-2CaOSiO 2The form of sosoloid exists, and composes with metallic elements such as iron, manganese to be stored in the different mineral facies.Based on phosphorous phase and without phosphorus mutually huge magnetic properties difference, the effect that separates phosphoric can be played in the magnetic field that applies certain intensity.But because phosphorous phase disperse distributes in the dephosphorized slag, tight with without phosphorus phase embedding cloth, in order to reach isolating purpose, so add properties-correcting agent, properties-correcting agent and dephosphorized slag mixture are reacted under molten state, and change dephosphorized slag thing phase composite and element distributes, make phosphoric in the slag be enriched in one or the one group of stable mineral.Cooling and broken back adopt magnetic separation to separate again.Reached the purpose of from converter duplex dephosphorized slag, separating and reclaim phosphoric effectively.
As optimization, the properties-correcting agent of adding is one or more in quartz sand, river sand, cullet, flyash, bauxitic clay and the titanium slag.These are common material, possess the cheap advantage of cost.When implementing certainly, also can choose other and be rich in SiO 2, Al 2O 3And TiO 2Raw material; Perhaps other acidity or neutral oxide, selection principle are to make it easily and 3CaOP 2O 5-2CaOSiO 2In CaO and SiO 2Reaction is rich in P thereby make 2O 5Rich phosphorus by independent.
As optimization, SiO in dephosphorized slag and the properties-correcting agent mixture 2, Al 2O 3And TiO 2Total amount control by 25～40% of gross weight.This ratio is to obtain by material proportion content and the reactive chemistry formula of analyzing in the general dephosphorized slag, adopts this ratio can make by reaction and will be rich in P 2O 5The mutually independent effect of rich phosphorus reach best.During actual enforcement, can adjust concrete ratio as the case may be.
As optimization, during to the mixture cooling after the high-temperature fusion processing, initial cooling temperature can guarantee the flowability of slag more fully more than 1500 ℃, promotes separating of phosphorus and iron.Initial cooling temperature is better greater than 1600 ℃ of effects.During cooling more than 1200 ℃ the temperature range cooling rate smaller or equal to 10 ℃/min.This cooling rate can promote the mineral grain growth, helps improving the later separation effect, and cooling rate can make effect better less than 5 ℃/min.Temperature during less than 1200 ℃ naturally cooling get final product.According to 3CaOP 2O 5-CaF 2Phasor, painstakingly reduce speed of cooling and generate β-C on the contrary easily this moment 3The P phase has reduced P in the slag 2O 5The molten rate of Chinese holly, the fertilizer efficiency that reclaims the thomas phosphate that slag makes is reduced.Like this, can change the slag phase structure, make it help the later separation step more, improve separating effect by the means of control dephosphorized slag condensation process.
As optimization, condensed mixture slag specimen is crushed to below the 20mm, and is finely ground in ball mill below 300 orders.Like this, can make rich phosphorus more abundant with separating of without phosphorus phase mutually.
Say that in further detail the present invention has provided a kind of mode that reclaims by slag modification+magnetic separation, phosphoric in the converter duplex dephosphorized slag is carried out the method for effective Separation and Recovery, described method comprises following concrete steps:
1) adds properties-correcting agent
Add that acidity or neutral oxide change dephosphorized slag thing phase composite and element distributes, phosphoric in the slag is enriched in one or the one group of stable mineral.Can adopt quartz sand, river sand, cullet, flyash, bauxitic clay and titanium slag etc. to be rich in SiO 2, Al 2O 3And TiO 2Raw material make properties-correcting agent.SiO in dephosphorized slag and the properties-correcting agent mixture 2, Al 2O 3And TiO 2Total amount control by 25～40% of gross weight.Add SiO 2After the modification, lower basicity makes the 2CaOSiO in the slag 2And 2CaOFe 2O 3Can not stable existence, generation the mineral with the relatively lower form of Ca/Si occur.Phosphorus enters rich phosphorus phase Ca 3[(P, Si) O 4] 2, iron mainly exists mutually with RO, and is more easily separated.Add Al 2O 3After the modification, 3CaOP 2O 5-2CaOSiO 2Portion C aO in the sosoloid and SiO 2Captured, generated Ca 2Al 2SiO 7, make the further enrichment of phosphorus.Add TiO 2After the modification, generate CaTiSiO 5Deng material, make the further enrichment of phosphorus equally.In addition, add a certain amount of above-mentioned substance and can reduce Tc in slag viscosity and the process of cooling, promote the mass transfer of phosphorus in liquid slag.
2) fusion cooling
Will be extremely liquid in changing slag hearth by the mixture melt that dephosphorized slag and properties-correcting agent are formed.At high-temperature zone insulation certain hour, be collected in the slag top to guarantee the less phosphorous come-up mutually of density, and Fe 2O 3Sink down into the slag bottom gradually with the bigger material of MnO isodensity.Initial cooling temperature requires more than 1500 ℃, and is better greater than 1600 ℃.Change the slag phase structure by control dephosphorized slag condensation process.The temperature range cooling rate is smaller or equal to 10 ℃/min, to promote the mineral grain growth more than 1200 ℃.Cooling rate is better less than 5 ℃/min effect.But temperature naturally cooling during less than 1200 ℃ is to reduce the β-C of the low molten rate of Chinese holly 3The generation probability of P.
3) broken ball milling
With crusher condensed slag is crushed to below the 20mm, in ball mill, is finely ground to below 300 orders, to guarantee fully separating of rich phosphorus phase and without phosphorus phase.
4) magnetic separation separates
Adopt the mode of magnetic separation to separate the nonmagnetics of rich phosphorus and the magnetic thing of Fu Tie, the rich phosphorus of recovery is as the agricultural phosphate fertilizer raw material.
Acidity or neutral oxide are tiny to mineral crystal grain by adding among the present invention, the disperse of iron phosphorus distributes, rich phosphorus mutually and rich iron phase embedding cloth closely dephosphorized slag carry out modification, the occurrence form of phosphorus in slag changed and reach the effect of enrichment, handle through magnetic separation again and reclaim rich phosphorus phase.So the present invention has realized that the resource utilization of phosphoric reclaims in the dephosphorized slag, the middle mutually phosphorus content of the rich phosphorus of recovery is higher, through further handling, can be used for producing thomas phosphate, promotes the recycling of bessemer furnace slag at agriculture field.In addition, by treatment process provided by the invention, also recyclable low-phosphorous rich iron phase returns converter and uses, so just turn waste into wealth, solve dephosphorized slag fully and taken good farmland, problem of environment pollution caused, reduced the converter supplementary product onsumption simultaneously, improved the converter recovery rate of iron.The present invention provides a kind of new metallurgical slag recycling thinking for the public.Simultaneously, it is simple that the present invention also possesses method, and it is convenient to implement, and implementation cost is cheap, advantages such as good separating effect.
Embodiment
Below in conjunction with embodiment and experimental data content of the present invention and effect are described in further detail.
Embodiment 1:
In the present embodiment, adopt the method for simulation test, content of the present invention and effect are done further checking.Comprise following processing step during enforcement:
1) the simulation slag of the mixture of properties-correcting agent and dephosphorized slag is packed into MgO crucible is inserted in the 12kW resistance furnace;
2) be warming up to 1550 ℃ and time insulation half an hour with stove, slag fully melted evenly, assurance 3CaOP 2O 5-2CaOSiO 2Sosoloid fully floats;
3) reduce to 1350 ℃ with the speed of 10 ℃/min, insulation 120min fully promotes 3CaOP 2O 5Separate out, reduce to 1200 ℃ with the speed of 10 ℃/min again, slag specimen is taken out, air cooling is to room temperature;
4) with condensed slag specimen fragmentation, below ball milling to 300 order;
5) with the magnetic separation pipe granulated slag being carried out magnetic separation separates.
Specifically, during test, in above-mentioned steps, be according to the industrial slag composition, adopt analytical reagent preparation simulation slag to represent the mixture of industrial slag and properties-correcting agent.With the P in the slag 2O 5Content is fixed as 10% with high phosphorus hot metal converter duplex smelting dephosphorized slag in the simulation.Simulation slag component sees Table 1.Wherein, No. 1 slag specimen is simulated the situation that independent industrial dephosphorized slag does not add properties-correcting agent; Al is added in 2, No. 3 slag specimen simulations 2O 3Situation when making properties-correcting agent; SiO is added in 4, No. 5 slag specimen simulations 2Situation when making properties-correcting agent; TiO is added in No. 6 slag specimen simulations 2Situation when making properties-correcting agent; 7, No. 8 slag specimens are simulated respectively and are added weakly alkaline oxide M nO and Fe 2O 3The situation of making properties-correcting agent as a comparison case.
Table 1 simulation slag ingredient (wt%)
Figure GSA00000124134400061
The weight ratio of phosphorus is the partition ratio of phosphorus in phosphorus after the definition magnetic separation in the nonmagnetics and the magnetic thing.%M and %N represent the weight percent of magnetic thing and nonmagnetics after the magnetic separation respectively in the formula; (P) and [P] represent phosphorus content in nonmagnetics and the magnetic thing respectively.
L p = % N × ( P ) % M × [ P ]
According to aforementioned implementation step, be 300 orders in the slag specimen granularity, magnetic separation pipe magneticstrength is under the condition of 2800Oe, the magnetic separation result is as shown in table 2.No. 1 slag phosphor partition ratio of simulation actual industrial slag is 0.6 only, and the phosphorus element content in the nonmagnetics even be lower than in the magnetic thing illustrate that only depending on magnetic separation to handle dephosphorized slag can't obtain effect as the conventional converter slag of processing.Add acidity or neutral modification agent SiO 2, Al 2O 3And TiO 2After, phosphor partition ratio can increase considerably, and makes that most phosphorus concentrate in the nonmagnetics in the slag, and phosphor partition ratio increases with the increase of properties-correcting agent ratio.With weakly alkaline oxide M nO and Fe 2O 3Make the flowability that properties-correcting agent can improve molten slag, promote the mass transfer of phosphoric, but its increase effect to phosphor partition ratio is limited to rich phosphorus phase.
Table 2 magnetic separation result
Figure GSA00000124134400071
Embodiment 2
Adopt industrial dephosphorized slag, its composition is as shown in table 3.Adopt SiO respectively 2And Al 2O 3Make properties-correcting agent industrial slag is carried out the modification processing, add 10% P 2O 5Smelt dephosphorized slag with high phosphorus hot metal converter duplex in the simulation.The enforcement parameter is as shown in table 4.Processing step is consistent with embodiment 1 during enforcement.
The industrial dephosphorized slag composition of table 3 (wt%)
Table 4 industrial slag modified component weight ratio
Figure GSA00000124134400073
Magnetic separation is the result show: work as SiO 2When making properties-correcting agent, phosphor partition ratio is 2.53, and 72% phosphoric is recycled in the nonmagnetics in the dephosphorized slag; Al when equivalent 2O 3When making properties-correcting agent, phosphor partition ratio is up to 7.14, and 88% phosphoric is recycled in the nonmagnetics in the dephosphorized slag.The magnetic separation result has proved the feasibility of the inventive method.
The foregoing description magnetic separation is the result also find: CaO, SiO 2, P 2O 5And TiO 2Mainly be enriched in the nonmagnetics, and Fe 2O 3, MnO, MgO and Al 2O 3Then mainly be present in the magnetic substance.So, also the low-phosphorous magnetic substance that is rich in elements such as iron, manganese can be returned converter and use by the valuable element phosphorus in the not only recyclable dephosphorized slag of separating technology provided by the invention, improve recovery rate of iron, reduce production costs.The embodiment of the invention is not taked stir process, stirs if increase in the slag system, can improve the dynamic conditions of slag element mass transfer, can obtain more excellent result of implementation.

Claims (6)

1. the recovery method of phosphoric in the converter duplex dephosphorized slag is characterized in that: add acidity or neutral oxide as properties-correcting agent in dephosphorized slag; The mixture of dephosphorized slag and properties-correcting agent is carried out high-temperature fusion handle, make properties-correcting agent change dephosphorized slag thing phase composite and element distributes, make phosphoric in the slag be enriched in one or the one group of stable mineral; To the mixture cooling after the above-mentioned high-temperature fusion processing, cooled mixture carries out magnetic separation behind fragmentation, ball milling separates, and obtains the nonmagnetics of rich phosphorus and low-phosphorous magnetic thing.
2. the recovery method of phosphoric is characterized in that in the converter duplex dephosphorized slag according to claim 1, and the properties-correcting agent of adding is one or more in quartz sand, river sand, cullet, flyash, bauxitic clay and the titanium slag.
3. the recovery method of phosphoric is characterized in that in the converter duplex dephosphorized slag according to claim 1, SiO in dephosphorized slag and the properties-correcting agent mixture 2, Al 2O 3And TiO 2Total amount control by 25～40% of gross weight.
4. the recovery method of phosphoric in the converter duplex dephosphorized slag according to claim 1, it is characterized in that, during to the mixture cooling after the high-temperature fusion processing, initial cooling temperature is more than 1500 ℃, and the temperature range cooling rate is smaller or equal to 10 ℃/min more than 1200 ℃.
5. the recovery method of phosphoric in the converter duplex dephosphorized slag according to claim 4, it is characterized in that, during to the mixture cooling after the high-temperature fusion processing, initial cooling temperature is more than 1600 ℃, and the temperature range cooling rate is less than 5 ℃/min more than 1200 ℃.
6. the recovery method of phosphoric is characterized in that in the converter duplex dephosphorized slag according to claim 1, and condensed mixture slag specimen is crushed to below the 20mm, and is finely ground in ball mill below 300 orders.
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102517416A (en) * 2011-12-30 2012-06-27 重庆大学 Efficient dephosphorizing agent based on refined steel ladle after-cast recovery slag for revolving furnace
CN104141018A (en) * 2014-07-23 2014-11-12 重庆大学 Recycling method for steel slag
CN104294003A (en) * 2014-09-24 2015-01-21 王虎 Modification technology for steel slag in converter dephosphorization stage
CN104561404A (en) * 2015-01-06 2015-04-29 北京科技大学 Method for preparing phosphate enriched phase by using steelmaking slag
CN104711391A (en) * 2015-03-27 2015-06-17 青岛钢铁控股集团有限责任公司 Method for separating phosphorus in converter slag and recycling converter slag
JP2015526588A (en) * 2012-06-12 2015-09-10 サントル ナスィオナル ド ラ ルシェルシュ スィアンティフィク（セ．エン．エル．エス．） Processing method of converter slag
CN105714004A (en) * 2014-12-01 2016-06-29 鞍钢股份有限公司 Treatment method of converter final slag
CN109897934A (en) * 2019-02-28 2019-06-18 钢铁研究总院 A method of improving phosphorus efficiency concentration effect in phosphorous steel slag
CN111893228A (en) * 2020-07-31 2020-11-06 钢铁研究总院 P in phosphorus-containing steel slag is improved2O5Method for improving citric acid solubility
CN114472464A (en) * 2022-01-14 2022-05-13 江苏大学 Method for efficiently recycling iron and phosphorus resources in phosphorus-containing steel slag

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102517416A (en) * 2011-12-30 2012-06-27 重庆大学 Efficient dephosphorizing agent based on refined steel ladle after-cast recovery slag for revolving furnace
JP2015526588A (en) * 2012-06-12 2015-09-10 サントル ナスィオナル ド ラ ルシェルシュ スィアンティフィク（セ．エン．エル．エス．） Processing method of converter slag
CN104141018B (en) * 2014-07-23 2016-08-10 重庆大学 A kind of slag recoverying and utilizing method
CN104141018A (en) * 2014-07-23 2014-11-12 重庆大学 Recycling method for steel slag
CN104294003A (en) * 2014-09-24 2015-01-21 王虎 Modification technology for steel slag in converter dephosphorization stage
CN104294003B (en) * 2014-09-24 2019-07-09 王虎 A kind of converter in stage steel slag modification technique
CN105714004A (en) * 2014-12-01 2016-06-29 鞍钢股份有限公司 Treatment method of converter final slag
CN104561404A (en) * 2015-01-06 2015-04-29 北京科技大学 Method for preparing phosphate enriched phase by using steelmaking slag
CN104711391B (en) * 2015-03-27 2016-08-17 青岛钢铁控股集团有限责任公司 A kind of method that phosphorus in vessel slag was separated and recycled vessel slag
CN104711391A (en) * 2015-03-27 2015-06-17 青岛钢铁控股集团有限责任公司 Method for separating phosphorus in converter slag and recycling converter slag
CN109897934A (en) * 2019-02-28 2019-06-18 钢铁研究总院 A method of improving phosphorus efficiency concentration effect in phosphorous steel slag
CN111893228A (en) * 2020-07-31 2020-11-06 钢铁研究总院 P in phosphorus-containing steel slag is improved2O5Method for improving citric acid solubility
CN114472464A (en) * 2022-01-14 2022-05-13 江苏大学 Method for efficiently recycling iron and phosphorus resources in phosphorus-containing steel slag

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