CN102674470A - Method for purifying ferric oxide red by wet method - Google Patents
Method for purifying ferric oxide red by wet method Download PDFInfo
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Abstract
The invention aims to provide a method for purifying ferric oxide red by a wet method. The method comprises the process route of water-washing, dehydrating and drying and is characterized in that an additive with the ammonia content of 0.05 to 35 percent is added in the water-washing process; impurities are separated by a centrifugal dehydrator during dehydration; preferably, the additive can be ammonia, ammonia water, ammonium carbonate or ammonium hydrogen carbonate with the ammonia content of 0.05 to 35 percent; and the drying method is rotary kiln drying or pulping-centrifugal spraying drying. High-quality ferric oxide powder is obtained by purifying the ferric oxide powder and can serve as a raw material of a high-end product with high magnetic conductivity.
Description
Technical field
The present invention relates to a kind of red iron oxide method of purification, a kind of iron oxide powder solid purifying process that utilizes wet processing is provided especially.
Background technology
1, the performance requriements of manganese-zinc ferrite body and function red stone
From the nineties in last century, the world transfers to China in the soft magnetic ferrite production center gradually.According to statistics, national soft magnetic ferrite output in 2000 is about 60,000 tons.
Homemade soft magnetic ferrite occupies significant proportion in global low-and-medium-grade products, but the market share in expensive goods is far below developed countries such as day, Europe.Wherein, starting material are conspicuous to the restriction of Chinese soft magnetic ferrite quality.The weight percent of red stone is about 70% in the Mn-Zn ferrite raw material, so will make high-grade Mn-Zn ferrite, raw iron oxide material must satisfy corresponding performance requriements.
2, the production technique of red stone
In the pressure water on modern rolling steel production, generally use hydrochloric acid that hot-rolled steel sheet is carried out pickling, cool off after the removal zone of oxidation again, the spent pickle liquor staple is FeC1
2, generating HC1 gas through thermal degradation, water-soluble regeneration salt acid recovery is used, and obtains the sub product red stone simultaneously.The Ruthner method is that first-selected acid recovery process is produced in modern steel rolling, and its main flow process is following: the acid fluid dissolves waste steel plate, and add ammoniacal liquor and improve acid solution pH value, the ventilation oxidation produces Fe (OH)
3Deposition will precipitate the condensation prod filtering, and the high purity acid solution of gained generates red stone through spray roasting again.The impurity of in the production process of red stone, introducing mainly contains Al, Cr, Na, P, Si, S, C1 etc.The pickling of some exotic materials such as autobody sheet also can be introduced B.In order to obtain the high-quality high purity ferric oxide, before and after roasting, must carry out the purification processing to spent pickle liquor and red stone respectively.
3, the performance of red stone is to manganese-zinc ferrite powder technology and Effect on Performance
3.1 the chemical property of red stone
The purity of red stone is the primary factor that influences the Mn-Zn ferrite performance, and the impurity in the red stone mainly shows as the improper growth that influences crystal grain to ferritic influence, causes the character defective, thereby influences ferritic microtexture and intrinsic characteristic.Wherein, Si and Cl, S content are quite crucial.Adding a small amount of Si during pulverizing is of great benefit to improving the Mn-Zn ferrite performance, yet inherent Si but has a strong impact on ferrite performance in the red stone.Acid group such as C1, S element at high temperature can volatilize, and easy etching apparatus and contaminate environment, seriously restricts the Mn-Zn ferrite production technique, and performance is had a negative impact.Table l has enumerated the physical and chemical index of domestic and international part quality oxide iron.
3.2 the physicals of red stone
In actual ferrite production, the starting material that chemical ingredients is good sometimes may not necessarily obtained performance and the good ferrite of microtexture, and its reason is exactly the influence of physicals.The physicals of the red stone that table 1 is listed comprises median size APS, specific surface area SSA and loose density BD.
Because red stone accounts for about 70% in the Mn-Zn ferrite prescription, so its APS value has great influence to the APS value of ferrite powder.In general, red stone APS value is little, and the APS value of ferrite powder is also little, helps accelerating the speed of chemical reaction.Yet consider that meticulous compacting of road, back and the sintering of being unfavorable for of powder particle is prone to the crystalline situation, the APS value is unsuitable too small.Obviously, when red stone APS value is excessive, when pre-burning,, only can carry out the diffusion reaction of spinel phase, can't further carry out grain growth process because particle diameter is bigger.Intensity of activation required when this must cause sintering improves, and is unfavorable for solid state reaction.
Secondly, in general, croci is thin, and promptly specific surface area SSA value is big, and reactive behavior is good, under certain processing condition, obtains the fine iron oxysome easily.But meticulous powder is reunited easily, brings difficulty for the batch mixing homogeneity.And fine powder very easily causes in sintering process and forms big single component granule from sintering, causes ferrite performance to worsen.Nano raw material just had a strong impact on its application in the Mn-Zn soft magnetic ferrite industry from sintering.As far as spheroidal particle, the SSA value is big, and then the APS value is little.But it is, not necessarily like this as far as irregularly shaped particles.
Loose density BD is a comprehensive parameters.Generally, the APS value is little, and the SSA value is big, and then BD is little.Because intergranular friction has increased.Simultaneously, BD has also reflected coating of particles, and particle shape is irregular more, and sphericity is low more, and then BD is just more little.Research shows that spheroidal particle has better activity than rod particle.
The acquisition of steel mill's solid oxidation iron powder mainly is that spent pickle liquor is handled; Generate through spray roasting; Present domestic this employing of the present RUTHNER sinter process, for obtaining purer high-quality brown iron oxide, spent pickle liquor carries out fluid purification (desilication process) before carrying out spray roasting.Along with lower end product iron oxysome to the improving constantly of the requirement of brown iron oxide, make it show out following two problems especially, 1, chemical index CL (chloride ion content) requirement that do not reach ultra-pure oxidation iron powder, and fluctuation is bigger, it is often referred to and is marked between 0.1 ~ 0.3%; Physical index BET (physicals) is on the low side, generally between 2.0 ~ 3.7/g, can not reach the requirement of producing high magnetic permeability red stone (downstream high-end product), and consistence is poor.
Summary of the invention
The purpose of this invention is to provide a kind of red iron oxide wet-process purification method, obtain high-quality brown iron oxide, can be used as the raw material of high-end product high magnetic permeability through brown iron oxide is purified.The technical problem that the present invention solved is: reduce the content of cl ions in the brown iron oxide, improve the brown iron oxide physical index and improve consistence.
The invention provides a kind of red iron oxide wet-process purification method, operational path is: washing, dehydration, drying is characterized in that: in water washing process, adding ammonia content is the additive of 0.05-35 ﹪, adopts centrifuge to carry out separating impurity during dehydration.Wherein additive is preferably ammonia, ammoniacal liquor, carbonic acid ammonia or the ammonium hydrogencarbonate that ammonia content is 0.05-35 ﹪.Drying means can be rotary kiln drying or slurrying-centrifugal spray drying.
Red iron oxide wet-process purification method provided by the invention; It is characterized in that: the working parameter scope of said centrifuge: 0-4500 rev/min of rotary drum maximum speed; Working speed 150-4500 rev/min commonly used; Best result leaves factor 2560G, suspension-s processing power 1-30 cubic meter/hour, maximum deslagging ability 0.1-1500 kilogram/hour.Water extracter is preferably the CF-1500I centrifuge.
Red iron oxide wet-process purification method provided by the invention; It is characterized in that: said water washing process is: brown iron oxide is sent in the dissolving axe; In the weight ratio of brown iron oxide and washing water is that the ratio of 1:1 ~ 10 is dissolved brown iron oxide, adds weight percent then and be 0.1% ~ 30% additive; It is 0-80 ℃ that slip is remained on temperature, and rotating speed is to stir under the 5-150 rev/min of condition, stirs 10-120 minute; Wherein washing water are de-salted water or pure water.
Red iron oxide wet-process purification method provided by the invention is characterized in that: the concrete process step of said purification is:
Step a: brown iron oxide is sent in the dissolving axe, is that the ratio of 1:1 ~ 10 is dissolved brown iron oxide in the weight ratio of brown iron oxide and washing water, adds weight percent then and be 0.1% ~ 30% additive; It is 0-80 ℃ that slip is remained on temperature, and rotating speed is to stir under the 5-150 rev/min of condition, stirs 10-120 minute; Wherein washing water are de-salted water or pure water;
Step b: slip is ground, making the solid particulate diameter is the 0.5-1.0 micron again, grinds the back and delivers to separating impurity in the water extracter to slip, with its solid-liquid separation;
Step c: the solid of separating is sent in the dissolution kettle, repeats step a, delivers to separating impurity in the water extracter to slip then, with its solid-liquid separation; Or directly carry out steps d (promptly containing the washing that water solubles content carries out to twice) according to brown iron oxide;
Steps d: the solid water cut of separating is 10%-55%, it is sent into carry out drying treatment in the moisture eliminator.
Red iron oxide wet-process purification method provided by the invention is characterized in that: in step b, c, send into the water extracter separating impurity to slip, with its solid-liquid separation, control is considered the back water cut less than 30%.
Red iron oxide wet-process purification method provided by the invention is characterized in that: when steps d is carried out drying treatment, make its brown iron oxide drying after water cut less than 0.3%.
What the present invention used in washing iron oxide red process is de-salted water or pure water, and de-salted water or pure water generally are acid, and pH value is between 4-7; After iron oxide red is dissolved in de-salted water or pure water; It is acid that mixture shows, red oxide of iron pH value less than 3 situation under, do not form deposition; Must be between 3-13, in order to make red oxide of iron form the deposition pH value so we have used additive.This additive can make the mixture PH of deionized water and iron oxide red remain between the 3-13, and does not influence the quality of iron oxide red.
We combine production practice to study the influence of red stone physicochemical property to ferrite ME and product performance, and sum up manganese-zinc ferrite body and function red stone and should possess physicochemical property listed in the table 2:
The physical and chemical index requirement of table 2 manganese-zinc ferrite body and function red stone
| ? | High purity | Moderate purity | Low-purity |
| Fe 2O 3/wt% | ≥99.4 | ≥99.2 | ≥98.5 |
| SiO 2/10 -6 | 80~150 | 150~350 | 300~500 |
| CaO/10 -6 | ≤200 | ≤400 | ≤500 |
| Al 2O 3/10 -6 | ≤200 | ≤400 | ≤600 |
| Oxide compound/10 -6 | ≤1000 | ≤1300 | ≤1500 |
| Sulfide/10 -6 | ≤300 | ≤600 | ≤700 |
| APS/μm | 0.6~0.8 | 0.7~0.9 | 0.7~0.9 |
| SSA/m 2·g -1 | 5 | 5 | 4~6 |
| BD/g·cm -3 | 0.45~0.6 | 0.4~0.45 | 0.4~0.6 |
Adopt technical process of the present invention that the solid oxidation iron powder is purified, its chemical property index of red stone and the physical performance index that obtains of purifying all is improved, and makes the quality of brown iron oxide can satisfy high-end ferritic ingredient requirement: Cl
-Smaller or equal to 0.6%, and make SO
4 2-, P
2O
5, K
2The decline in various degree of water-soluble micro impurity element such as O, PbO; BET can be increased to 4.0 ~ 5.5m2/g, and consistence obviously improves; Brown iron oxide after the solid purification processes can be as the raw material of high magnetic permeability red stone.
Description of drawings
Fig. 1 CF-1500I centrifuge working mechanism figure.
Embodiment
Embodiment 1
Step a: with the cold-rolling pickling iron oxide red in the storage tank; Be transported in the dissolution kettle via the measuring belt scale; According to cold-rolling pickling iron oxide red and deionized water is the ratio dissolving of 1:5, adds ammonia content and be 20% ammoniacal liquor as additive, and then slip being remained on temperature is 30 ℃; Rotating speed is 50 rev/mins and stirs, and stirs 20 minutes;
Step b: with ball mill slip is ground again; Keeping the solid particulate diameter is the 0.5-1.0 micron; Grind after deliver to separating impurity in the CF-1500I centrifuge (as shown in Figure 1) to slip by hose pump, with its solid-liquid separation, control is considered the back water cut less than 30%;
Step c: the liquid of separating is sent into tank, after treatment discharging.The solid of separating is sent in the dissolution kettle, carries out step a again, delivers to separating impurity in the CF-1500I centrifuge to slip via hose pump afterwards, and with its solid-liquid separation, control is considered the back water cut less than 30%;
Steps d: the liquid of separating is used for once washing.The solid water cut of separating is 10%-55%, it is sent into carry out drying treatment in the moisture eliminator, make its brown iron oxide drying after water cut less than 0.3%, packing is outer then sells.
The products obtained therefrom foreign matter content is few, and its physicochemical property test result is seen table 3.
Embodiment 2
Step a: with the cold-rolling pickling iron oxide red in the storage tank; Be transported in the dissolution kettle via the metering screw belt; According to cold-rolling pickling iron oxide red and deionized water is the ratio dissolving of 1:2, adds ammonia content and be 10% carbonic acid ammonia as additive, and then slip being remained on temperature is 50 ℃; Rotating speed is 20 rev/mins and stirs, and stirs 80 minutes;
Step b: with ball mill slip is ground, keeping the solid particulate diameter is the 0.5-1.0 micron again, grinds after deliver to separating impurity in the CF-1500I centrifuge to slip by hose pump, and with its solid-liquid separation, control is considered the back water cut less than 30%;
Step c: the liquid of separating is sent into tank, after treatment discharging.The solid of separating is sent in the dissolution kettle, carries out step a again, delivers to separating impurity in the CF-1500I centrifuge to slip via hose pump afterwards, and with its solid-liquid separation, control is considered the back water cut less than 30%;
Steps d: the liquid of separating is used for once washing.The solid water cut of separating is 10%-55%, it is sent into carry out drying treatment in the moisture eliminator, make its brown iron oxide drying after water cut less than 0.3%, packing is outer then sells.
The products obtained therefrom foreign matter content is few, and its physicochemical property test result is seen table 3.
Embodiment 3
Step a: with the cold-rolling pickling iron oxide red in the storage tank; Be transported in the dissolution kettle via the measuring belt scale; According to cold-rolling pickling iron oxide red and deionized water is the ratio dissolving of 1:9, adds ammonia content and be 5% ammonium hydrogencarbonate as additive, and then slip being remained on temperature is 20 ℃; Rotating speed is 100 rev/mins and stirs, and stirs 20 minutes;
Step b: with sand mill slip is ground, keeping the solid particulate diameter is the 0.5-1.0 micron again, grinds after deliver to separating impurity in the CF-1500I centrifuge to slip by hose pump, and with its solid-liquid separation, control is considered the back water cut less than 30%;
Step c: the liquid of separating is sent into tank, after treatment discharging.The solid of separating is sent in the dissolution kettle, carries out step a again, delivers to separating impurity in the CF-1500I centrifuge to slip via hose pump afterwards, and with its solid-liquid separation, control is considered the back water cut less than 30%;
Steps d: the liquid of separating is used for once washing.The solid water cut of separating is 10%-55%, it is sent into carry out drying treatment in the moisture eliminator, make its brown iron oxide drying after water cut less than 0.3%, packing is outer then sells.
The products obtained therefrom foreign matter content is few, and its physicochemical property test result is seen table 3.
Comparative Examples 1
Do not add additive, other step is with embodiment 1, and the products obtained therefrom foreign matter content is many, and its physicochemical property test result can't satisfy the listed requirement of table 2 (seeing table 3).
Comparative Examples 2
Do not add additive, other step is with embodiment 1, and the products obtained therefrom foreign matter content is many, and its physicochemical property test result can't satisfy the listed requirement of table 2 (seeing table 3).
The physical and chemical index of table 3 embodiment products obtained therefrom
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples 1 | Comparative Examples 2 |
| Fe 2O 3/wt% | 99.53 | 99.60 | 99.46 | 99.20 | 99.17 |
| SiO 2/10 -6 | 85 | 74 | 79 | 152 | 142 |
| CaO/10 -6 | 58 | 62 | 60 | 215 | 220 |
| Al 2O 3/10 -6 | 98 | 89 | 88 | 205 | 227 |
| Oxide compound/10 -6 | 980 | 990 | 990 | 2150 | 2200 |
| Sulfide/10 -6 | 244 | 220 | 258 | 560 | 630 |
| APS/μm | 2.77 | 0.71 | 0.80 | 0.85 | 0.81 |
| SSA/m 2·g -1 | 4.15 | 4.20 | 4.08 | 2.28 | 2.81 |
| BD/g·cm -3 | 0.55 | 0.54 | 0.57 | 0.62 | 0.50 |
Claims (8)
1. red iron oxide wet-process purification method, operational path is: washing, dehydration, drying is characterized in that: in water washing process, adding ammonia content is the additive of 0.05-35 ﹪, adopts centrifuge to carry out separating impurity during dehydration.
2. according to the said red iron oxide wet-process purification method of claim 1, it is characterized in that: said additive is ammonia, ammoniacal liquor, carbonic acid ammonia or ammonium hydrogencarbonate.
3. according to claim 1 or 2 said red iron oxide wet-process purification methods; It is characterized in that: the working parameter scope of said centrifuge: 0-4500 rev/min of rotary drum maximum speed; Working speed 150-4500 rev/min commonly used; Best result leaves factor 2560G, suspension-s processing power 1-30 cubic meter/hour, maximum deslagging ability 0.1-1500 kilogram/hour.
4. according to the said red iron oxide wet-process purification method of claim 3, it is characterized in that: said centrifuge is the CF-1500I centrifuge.
5. according to the said red iron oxide wet-process purification method of claim 1; It is characterized in that: said water washing process is: brown iron oxide is sent in the dissolving axe; In the weight ratio of brown iron oxide and washing water is that the ratio of 1:1 ~ 10 is dissolved brown iron oxide, adds weight percent then and be 0.1% ~ 30% additive; It is 0-80 ℃ that slip is remained on temperature, and rotating speed is to stir under the 5-150 rev/min of condition, stirs 10-120 minute; Wherein washing water are de-salted water or pure water.
6. according to the said red iron oxide wet-process purification method of claim 1, it is characterized in that: the concrete process step of said purification is:
Step a: brown iron oxide is sent in the dissolving axe, is that the ratio of 1:1 ~ 10 is dissolved brown iron oxide in the weight ratio of brown iron oxide and washing water, adds weight percent then and be 0.1% ~ 30% additive; It is 0-80 ℃ that slip is remained on temperature, and rotating speed is to stir under the 5-150 rev/min of condition, stirs 10-120 minute; Wherein washing water are de-salted water or pure water;
Step b: slip is ground, making the solid particulate diameter is the 0.5-1.0 micron again, grinds the back and delivers to separating impurity in the water extracter to slip, with its solid-liquid separation;
Step c: the solid of separating is sent in the dissolution kettle, repeats step a, delivers to separating impurity in the water extracter to slip then, with its solid-liquid separation; Or directly carry out steps d;
Steps d: the solid water cut of separating is 10%-55%, it is sent into carry out drying treatment in the moisture eliminator.
7. according to the said red iron oxide wet-process purification method of claim 6, it is characterized in that: in step b, c, send into the water extracter separating impurity to slip, with its solid-liquid separation, control is considered the back water cut less than 30%.
8. according to the said red iron oxide wet-process purification method of claim 6, it is characterized in that: when steps d is carried out drying treatment, make its brown iron oxide drying after water cut less than 0.3%.
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| CN105399143A (en) * | 2015-12-15 | 2016-03-16 | 上海宝钢磁业有限公司 | Iron oxide red for lithium iron phosphate and preparation method and application thereof |
| CN108695512A (en) * | 2018-06-14 | 2018-10-23 | 东北大学秦皇岛分校 | The acid washing iron red purposes as negative material |
| CN114031385A (en) * | 2021-10-22 | 2022-02-11 | 浙江安特磁材股份有限公司 | Method for preparing permanent magnetic ferrite material from high-chlorine iron oxide red |
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| CN114031385A (en) * | 2021-10-22 | 2022-02-11 | 浙江安特磁材股份有限公司 | Method for preparing permanent magnetic ferrite material from high-chlorine iron oxide red |
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