CN113943152A - Method for preparing permanent magnetic ferrite from high-chlorine iron oxide red and permanent magnetic ferrite - Google Patents
Method for preparing permanent magnetic ferrite from high-chlorine iron oxide red and permanent magnetic ferrite Download PDFInfo
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- CN113943152A CN113943152A CN202111038458.2A CN202111038458A CN113943152A CN 113943152 A CN113943152 A CN 113943152A CN 202111038458 A CN202111038458 A CN 202111038458A CN 113943152 A CN113943152 A CN 113943152A
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- iron oxide
- oxide red
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 60
- 239000000460 chlorine Substances 0.000 title claims abstract description 36
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 57
- 238000005245 sintering Methods 0.000 claims abstract description 43
- 238000000227 grinding Methods 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000006298 dechlorination reaction Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 69
- 239000000843 powder Substances 0.000 claims description 52
- 239000002002 slurry Substances 0.000 claims description 45
- 238000000498 ball milling Methods 0.000 claims description 44
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 40
- 239000002245 particle Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 238000001694 spray drying Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 238000000465 moulding Methods 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 13
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 12
- 239000004327 boric acid Substances 0.000 claims description 12
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical group O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 11
- 230000000996 additive effect Effects 0.000 claims description 11
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical group [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 11
- 235000013539 calcium stearate Nutrition 0.000 claims description 11
- 239000008116 calcium stearate Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000007780 powder milling Methods 0.000 claims description 10
- 229910052712 strontium Inorganic materials 0.000 claims description 10
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 6
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 13
- 238000004321 preservation Methods 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000009834 vaporization Methods 0.000 description 4
- 230000008016 vaporization Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000382 dechlorinating effect Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2683—Other ferrites containing alkaline earth metals or lead
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
Abstract
The invention relates to the field of magnetic materials, and discloses a method for preparing a permanent magnetic ferrite from high-chlorine iron oxide red and the permanent magnetic ferrite, which comprises the following steps: a) iron oxide red pretreatment, b) dechlorination, c) preparation of presintering raw material SrO.MFe2O3D) pre-burning, e) secondary grinding, f) sintering and the like. The scheme of the invention adopts high-chlorine iron oxide red as a raw material, so that the raw material source of the ferrite permanent magnet is widened; the preparation method is simple and can be suitable for large-scale production; the preparation process is green and environment-friendly, and the product performance is stable.
Description
Technical Field
The invention relates to the field of magnetic materials, in particular to a method for preparing a permanent magnetic ferrite from high-chlorine iron oxide red and the permanent magnetic ferrite.
Background
The production process of the iron oxide red, which is a main raw material for producing the permanent ferrite powder, has more routes, and is generally divided into a dry process and a wet process according to the state classification of reaction raw materials. The early development of the steel industry is mainly based on a dry method, and the iron oxide red required by the magnetic industry is mainly obtained by washing and calcining. The prior pickling treatment is carried out in the steel industry, the content of generated iron red hetero-ions is extremely high, and the pickling treatment is not friendly to the magnetic material industry. The prior patent technology mainly adopts iron scale and conventional iron oxide red as main materials for production, and the impurity content, particularly the impurity content of chlorine, silicon and the like, meets the use requirement of a permanent magnetic ferrite material. The acid-washed iron powder is difficult to be used as a production raw material in the prior art to produce high-end materials due to the high content of chloride ions.
The grant number is CN201410352413.6, and discloses a preparation process of a ferrite composite permanent magnet for a permanent magnet direct current motor, which takes FeCl2 as an iron oxide raw material to generate Fe (OH) in solution3And calcined to obtain iron oxide. Although the method relates to Cl element, the raw material of the method does not adopt acid-washing iron oxide red, and the technical problem proposed by the scheme is not solved.
The publication No. CN201210074240.7 discloses a novel method for dechlorinating iron oxide red by acid pickling, which uses steam as a catalyst and a multi-stage drying kiln as a heat source carrier, and makes chlorides in the acid-pickled iron oxide red react with the steam at about 400-500 ℃, and the chlorides are finally separated by a flue gas recovery system in the form of hydrogen chloride, thereby achieving the purpose of reducing the content of chloride ions in the iron oxide red. Although the chlorine content can be reduced to a certain extent by the scheme, the water vapor in the multi-stage drying kiln is difficult to control, and the technical difficulty is higher.
Disclosure of Invention
The invention aims to solve the problem that acid-washed iron powder is difficult to be used as a production raw material to produce high-end materials in the prior art due to high chloride ion content, and provides a method for preparing a permanent magnetic ferrite from high-chloride iron oxide red; the preparation method is simple and can be suitable for large-scale production; the preparation process is green and environment-friendly, and the product performance is stable.
The invention provides a method for preparing a permanent magnetic ferrite from high-chlorine iron oxide red, which comprises the following steps:
a) iron oxide red pretreatment: according to the proportion of 1: 0.5-1.0: mixing and ball-milling iron oxide red containing 0.15-0.3% of chlorine element, a solvent and a dispersant in a mass ratio of 0.0005-0.002 to obtain uniform slurry;
b) dechlorination: spray drying the slurry obtained in the step a) at the temperature of 100 ℃ and 300 ℃ to obtain a main material;
c) preparation of Pre-fired raw Material SrO.MFe2O3: mixing the main material and the auxiliary material obtained in the step b) according to the proportion M of 5.2-6.5, and then adding 0-6 wt% of the mixed materialAdding the additive A into ball milling liquid according to the mass ratio of 1:0.9-1.1, carrying out ball milling to obtain uniform powder, and then drying to obtain a pre-sintered raw material; the presintering raw material is SrO.MFe2O3The strontium ferrite mixture of (1);
d) pre-burning: sintering the pre-sintering raw material prepared in the step c) at 1200-;
e) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder, adding an additive B with the mass fraction of 0-6 wt% into the coarse powder, and ball-milling again to obtain fine slurry;
f) and (3) sintering: and e) pressing and molding the fine slurry obtained in the step e), and sintering at the temperature of 1200-1300 ℃ for 1-3 hours to obtain the permanent magnetic ferrite.
The scheme can prepare the high-performance ferrite by using the iron oxide red containing 0.15-0.3% of chlorine element. The iron oxide red pretreatment process in the step a) is ball-milled, so that the specific surface area of iron oxide red particles is improved, chlorine elements can be ensured to be dissolved into a solvent as far as possible, the uniformity of the iron oxide red particles is improved, and the dispersing agent is used for improving the dispersibility of the iron oxide red in water so as to facilitate better refinement of the iron oxide red and uniform dissolution of impurities; the dechlorination operation is carried out by spray drying in the step b), and the process of spraying the fog agent is a decompression process, which is favorable for the vaporization of the solvent and further promotes the vaporization of the solvent at the high temperature of 100 ℃ and 300 ℃. In the course of solvent vaporization, Cl-Complex physicochemical reactions can occur, such as when the solvent is deionized water: 1. in the course of the depressurization, Cl-With the original H in the solvent+Combine HCl and volatilize; 2. solvent vaporization to carry away Cl-(ii) a 3. Reacting the chlorine-containing salt with solvent steam to generate HCl and volatilizing the HCl; 4. the hydrolysis of the chloride-containing salt with the solvent produces HCl and is volatilized, etc. The additive A in the step c) has the functions of reducing the sintering temperature and improving the compactness of the material, and different M ratios can cause differences in final properties of products.
Preferably, in step a), the particle size of the homogeneous slurry is 1 to 1.5 μm; the solvent is deionized water; the dispersing agent is calcium stearate.
To make Cl-Can be sufficiently removed, the solvent selected in step a) is a deionized solventThe dispersant is calcium stearate. Controlling the particle size of the uniform slurry to be 1-1.5 μm can ensure the sufficient dissolution of chlorine element and guarantee the uniformity of the subsequent process.
Preferably, in step b), the chlorine content of the main material is 0.01-0.1 wt%.
The chlorine content in the raw materials can be reduced by a spray drying method, and the effect is better when the chlorine content of the main material can be controlled to be 0.001-0.01 wt%.
Preferably, in the step c), the ingredient is strontium carbonate; the additive A is one or more of silicon dioxide, aluminum oxide or calcium carbonate or boric acid; the ball milling liquid is water; the particle size of the uniform powder is 0.5-1.0 μm.
Preferably, in step d), the pre-burning process is performed in air; the sintering condition of the pre-sintering raw material is 1260-1300 ℃, and the temperature is kept for 1-2 hours.
Preferably, the particle size of the coarse powder is 3.5-5 μm; the additive B is one or a mixture of more of calcium carbonate, strontium carbonate, silicon dioxide, aluminum oxide and boric acid; the grain diameter of the fine slurry is 0.6-1.0 μm.
In order to make the incorporation of additive B more uniform, additive B is added at the time after the coarse powder grinding is completed. In order to ensure uniform magnetic and mechanical properties of the product, the fine slurry particles used to sinter the final product should be as fine as possible while reducing the sintering conditions.
Preferably, in step f), the method for press forming is a wet press forming method, which comprises the following steps:
1) standing and filtering the fine slurry obtained in the step e);
2) after water filtration, press forming is carried out, and simultaneously, a forming magnetic field of 9000-11000Oe is applied in the pressing direction.
The pressing process is carried out in a magnetic field, so that the orientation of crystal grains can be optimized, and the sintered finished product has better measuring performance.
Preferably, in step 2), the mold pressure is 3 to 5 MPa.
Preferably, in the step f), the sintering temperature is 1230-1260 ℃, and the heat preservation time is 1.5-2.5 hours.
The invention also provides a permanent magnetic ferrite prepared by any one of the methods.
The invention has the beneficial effects that:
1. the high-chlorine iron oxide red is used as a raw material, so that the raw material source of the ferrite permanent magnet is widened;
2. the preparation method is simple and can be suitable for large-scale production;
3. the preparation process is green and environment-friendly, and the product performance is stable.
Detailed Description
The present invention will be further described with reference to the following examples. The devices, reagents and methods referred to in the present invention are those known in the art unless otherwise specified.
Example 1:
a) iron oxide red pretreatment: according to the weight ratio of 1: 0.8: mixing and ball-milling iron oxide red containing 0.2 percent of chlorine element, deionized water and calcium stearate according to the mass ratio of 0.001 to obtain uniform slurry of 1.2 mu m;
b) dechlorination: spray drying the slurry obtained in the step a) at the temperature of 200 ℃ to obtain a main material, wherein the content of chloride ions in the main material is 0.09%;
c) preparation of Pre-fired raw Material SrO.MFe2O3: mixing the main material and the auxiliary material obtained in the step b) according to a proportion M of 5.9, then adding 0.2 wt% of calcium carbonate and 0.1% of alumina powder based on the mass of the mixed material, then adding water according to a mass ratio of 1:1, performing ball milling to obtain uniform powder, wherein the particle size of the uniform powder is 0.8 mu M, and then drying to obtain a pre-sintered raw material; the presintering raw material is SrO.5.9Fe2O3The strontium ferrite mixture of (1);
d) pre-burning: sintering the pre-sintered raw material prepared in the step c) in the air at 1270 ℃, and preserving heat for 1 hour to obtain a ferrite pre-sintered material;
e) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder with the particle size of 4 mu m, then adding 0.8 mass percent of calcium carbonate, 0.3 mass percent of strontium carbonate, 0.2 mass percent of silicon dioxide and 0.1 mass percent of boric acid into the coarse powder, and ball-milling again to obtain fine slurry with the particle size of 0.6 mu m;
f) and (3) sintering: and e) performing wet pressing molding on the fine slurry obtained in the step e) under the condition of 4MPa, and sintering at 1260 ℃ for 1.5 hours under the condition of heat preservation to obtain the permanent magnetic ferrite.
Example 2: (different from example 1 in the content of chlorine in the raw material iron oxide red)
a) Iron oxide red pretreatment: according to the weight ratio of 1: 0.8: mixing and ball-milling iron oxide red containing 0.3 percent of chlorine element, deionized water and calcium stearate according to the mass ratio of 0.001 to obtain uniform slurry of 1.2 mu m;
b) dechlorination: spray drying the slurry obtained in the step a) at the temperature of 200 ℃ to obtain a main material, wherein the content of chloride ions in the main material is 0.12%;
c) preparation of Pre-fired raw Material SrO.MFe2O3: mixing the main material and the auxiliary material obtained in the step b) according to a proportion M of 5.9, then adding 0.2 wt% of calcium carbonate and 0.1% of alumina powder based on the mass of the mixed material, then adding water according to a mass ratio of 1:1, performing ball milling to obtain uniform powder, wherein the particle size of the uniform powder is 0.8 mu M, and then drying to obtain a pre-sintered raw material; the presintering raw material is SrO.5.9Fe2O3The strontium ferrite mixture of (1);
d) pre-burning: sintering the pre-sintered raw material prepared in the step c) in the air at 1270 ℃, and preserving heat for 1 hour to obtain a ferrite pre-sintered material;
e) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder with the particle size of 4 mu m, then adding 0.8 mass percent of calcium carbonate, 0.3 mass percent of strontium carbonate, 0.2 mass percent of silicon dioxide and 0.1 mass percent of boric acid into the coarse powder, and ball-milling again to obtain fine slurry with the particle size of 0.6 mu m;
f) and (3) sintering: and e) performing wet pressing molding on the fine slurry obtained in the step e) under the condition of 4MPa, and sintering at 1260 ℃ for 1.5 hours under the condition of heat preservation to obtain the permanent magnetic ferrite.
Example 3: (different from example 1 in the content of chlorine in the raw material iron oxide red)
a) Iron oxide red pretreatment: according to the weight ratio of 1: 0.8: mixing and ball-milling iron oxide red containing 0.15 percent of chlorine element, deionized water and calcium stearate according to the mass ratio of 0.001 to obtain uniform slurry of 1.2 mu m;
b) dechlorination: spray drying the slurry obtained in the step a) at the temperature of 200 ℃ to obtain a main material, wherein the content of chloride ions in the main material is 0.05%;
c) preparation of Pre-fired raw Material SrO.MFe2O3: mixing the main material and the auxiliary material obtained in the step b) according to a proportion M of 5.9, then adding 0.2 wt% of calcium carbonate and 0.1% of alumina powder based on the mass of the mixed material, then adding water according to a mass ratio of 1:1, performing ball milling to obtain uniform powder, wherein the particle size of the uniform powder is 0.8 mu M, and then drying to obtain a pre-sintered raw material; the presintering raw material is SrO.5.9Fe2O3The strontium ferrite mixture of (1);
d) pre-burning: sintering the pre-sintered raw material prepared in the step c) in the air at 1270 ℃, and preserving heat for 1 hour to obtain a ferrite pre-sintered material;
e) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder with the particle size of 4 mu m, then adding 0.8 mass percent of calcium carbonate, 0.3 mass percent of strontium carbonate, 0.2 mass percent of silicon dioxide and 0.1 mass percent of boric acid into the coarse powder, and ball-milling again to obtain fine slurry with the particle size of 0.6 mu m;
f) and (3) sintering: and e) performing wet pressing molding on the fine slurry obtained in the step e) under the condition of 4MPa, and sintering at 1260 ℃ for 1.5 hours under the condition of heat preservation to obtain the permanent magnetic ferrite.
Example 4: (different from example 1 in that the spray drying temperature in step b) was different)
a) Iron oxide red pretreatment: according to the weight ratio of 1: 0.8: mixing and ball-milling iron oxide red containing 0.2 percent of chlorine element, deionized water and calcium stearate according to the mass ratio of 0.001 to obtain uniform slurry of 1.2 mu m;
b) dechlorination: spray drying the slurry obtained in the step a) at the temperature of 100 ℃ to obtain a main material, wherein the content of chloride ions in the main material is 0.11%;
c) preparation of Pre-fired raw Material SrO.MFe2O3: mixing the main material and the auxiliary material obtained in the step b) according to a proportion M of 5.9, then adding 0.2 wt% of calcium carbonate and 0.1% of alumina powder based on the mass of the mixed material, then adding water according to a mass ratio of 1:1, performing ball milling to obtain uniform powder, wherein the particle size of the uniform powder is 0.8 mu M, and then drying to obtain a pre-sintered raw material; the presintering raw material is SrO.5.9Fe2O3The strontium ferrite mixture of (1);
d) pre-burning: sintering the pre-sintered raw material prepared in the step c) in the air at 1270 ℃, and preserving heat for 1 hour to obtain a ferrite pre-sintered material;
e) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder with the particle size of 4 mu m, then adding 0.8 mass percent of calcium carbonate, 0.3 mass percent of strontium carbonate, 0.2 mass percent of silicon dioxide and 0.1 mass percent of boric acid into the coarse powder, and ball-milling again to obtain fine slurry with the particle size of 0.6 mu m;
f) and (3) sintering: and e) performing wet pressing molding on the fine slurry obtained in the step e) under the condition of 4MPa, and sintering at 1260 ℃ for 1.5 hours under the condition of heat preservation to obtain the permanent magnetic ferrite.
Example 5: (different from example 1 in that the spray drying temperature in step b) was different)
a) Iron oxide red pretreatment: according to the weight ratio of 1: 0.8: mixing and ball-milling iron oxide red containing 0.2 percent of chlorine element, deionized water and calcium stearate according to the mass ratio of 0.001 to obtain uniform slurry of 1.2 mu m;
b) dechlorination: spray drying the slurry obtained in the step a) at 300 ℃ to obtain a main material, wherein the content of chloride ions in the main material is 0.06%;
c) preparation of Pre-fired raw Material SrO.MFe2O3: mixing the main material and the auxiliary material obtained in the step b) according to a proportion M of 5.9, then adding 0.2 wt% of calcium carbonate and 0.1% of alumina powder based on the mass of the mixed material, then adding water according to a mass ratio of 1:1, performing ball milling to obtain uniform powder, wherein the particle size of the uniform powder is 0.8 mu M, and then drying to obtain a pre-sintered raw material; the presintering raw material is SrO.5.9Fe2O3The strontium ferrite mixture of (1);
d) pre-burning: sintering the pre-sintered raw material prepared in the step c) in the air at 1270 ℃, and preserving heat for 1 hour to obtain a ferrite pre-sintered material;
e) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder with the particle size of 4 mu m, then adding 0.8 mass percent of calcium carbonate, 0.3 mass percent of strontium carbonate, 0.2 mass percent of silicon dioxide and 0.1 mass percent of boric acid into the coarse powder, and ball-milling again to obtain fine slurry with the particle size of 0.6 mu m;
f) and (3) sintering: and e) performing wet pressing molding on the fine slurry obtained in the step e) under the condition of 4MPa, and sintering at 1260 ℃ for 1.5 hours under the condition of heat preservation to obtain the permanent magnetic ferrite.
Example 6: (different from example 1 in that M value in step c) is different)
a) Iron oxide red pretreatment: according to the weight ratio of 1: 0.8: mixing and ball-milling iron oxide red containing 0.2 percent of chlorine element, deionized water and calcium stearate according to the mass ratio of 0.001 to obtain uniform slurry of 1.2 mu m;
b) dechlorination: spray drying the slurry obtained in the step a) at 300 ℃ to obtain a main material, wherein the content of chloride ions in the main material is 0.06%;
c) preparation of Pre-fired raw Material SrO.MFe2O3: mixing the main material and the auxiliary material obtained in the step b) according to the proportion M of 6.2, then adding 0.2 wt% of calcium carbonate and 0.1% of alumina powder based on the mass of the mixed material, then adding water according to the mass ratio of 1:1, performing ball milling to obtain uniform powder, wherein the particle size of the uniform powder is 0.8 mu M, and then drying to obtain a pre-sintered raw material; the presintering raw material is SrO.5.9Fe2O3The strontium ferrite mixture of (1);
d) pre-burning: sintering the pre-sintered raw material prepared in the step c) in the air at 1270 ℃, and preserving heat for 1 hour to obtain a ferrite pre-sintered material;
e) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder with the particle size of 4 mu m, then adding 0.8 mass percent of calcium carbonate, 0.3 mass percent of strontium carbonate, 0.2 mass percent of silicon dioxide and 0.1 mass percent of boric acid into the coarse powder, and ball-milling again to obtain fine slurry with the particle size of 0.6 mu m;
f) and (3) sintering: and e) performing wet pressing molding on the fine slurry obtained in the step e) under the condition of 4MPa, and sintering at 1260 ℃ for 1.5 hours under the condition of heat preservation to obtain the permanent magnetic ferrite.
Comparative example 1: (different from example 1 in that spray drying treatment was not conducted)
a) Preparation of Pre-fired raw Material SrO.MFe2O3: mixing and ball-milling a main material (iron oxide red containing 0.2% of chlorine element, deionized water and calcium stearate in a mass ratio of 1: 0.8: 0.001) and an auxiliary material according to a proportion M of 5.9, then adding 0.2 wt% of calcium carbonate and 0.1% of alumina powder in the mass ratio of the mixture, then adding water in the mass ratio of 1:1, ball-milling to obtain uniform powder, wherein the particle size of the uniform powder is 0.8 mu M, and then drying to obtain a pre-sintering raw material; the presintering raw material is SrO.5.9Fe2O3The strontium ferrite mixture of (1);
b) pre-burning: sintering the pre-sintered raw material prepared in the step c) in the air at 1270 ℃, and preserving heat for 1 hour to obtain a ferrite pre-sintered material;
c) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder with the particle size of 4 mu m, then adding 0.8 mass percent of calcium carbonate, 0.3 mass percent of strontium carbonate, 0.2 mass percent of silicon dioxide and 0.1 mass percent of boric acid into the coarse powder, and ball-milling again to obtain fine slurry with the particle size of 0.6 mu m;
d) and (3) sintering: and e) performing wet pressing molding on the fine slurry obtained in the step e) under the condition of 4MPa, and sintering at 1260 ℃ for 1.5 hours under the condition of heat preservation to obtain the permanent magnetic ferrite.
Comparative example 2: (different from example 1 in that low-chlorine iron oxide red is used)
a) Preparation of Pre-fired raw Material SrO.MFe2O3: mixing and ball-milling a main material (iron oxide red containing 0.05% of chlorine element, deionized water and calcium stearate in a mass ratio of 1: 0.8: 0.001) and an auxiliary material according to a proportion M of 5.9, then adding 0.2 wt% of calcium carbonate and 0.1% of alumina powder in the mass ratio of the mixture, then adding water in the mass ratio of 1:1, ball-milling to obtain uniform powder, wherein the particle size of the uniform powder is 0.8 mu M, and then drying to obtain a pre-sintering raw material; the presintering raw material is SrO.5.9Fe2O3The strontium ferrite mixture of (1);
b) pre-burning: sintering the pre-sintered raw material prepared in the step c) in the air at 1270 ℃, and preserving heat for 1 hour to obtain a ferrite pre-sintered material;
c) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder with the particle size of 4 mu m, then adding 0.8 mass percent of calcium carbonate, 0.3 mass percent of strontium carbonate, 0.2 mass percent of silicon dioxide and 0.1 mass percent of boric acid into the coarse powder, and ball-milling again to obtain fine slurry with the particle size of 0.6 mu m;
d) and (3) sintering: and e) performing wet pressing molding on the fine slurry obtained in the step e) under the condition of 4MPa, and sintering at 1260 ℃ for 1.5 hours under the condition of heat preservation to obtain the permanent magnetic ferrite.
The properties and components of the products obtained are shown in Table 1.
TABLE 1
Through the embodiment 1 and the comparative example 1, the content of iron oxide red chloride ions treated is obviously reduced, the particle size of fine grinding slurry is improved, the activity of the material is improved, and the reaction area is increased, so that the performance of the material is improved; comparing examples 1,3 and 4, it can be seen that the content of chloride ions tends to decrease with the increase of the temperature of spray drying, which shows that the increase of the temperature is beneficial to further reducing the chloride ions in the raw materials; comparing example 5 with comparative example 2, it can be seen that the permanent magnet ferrite prepared by the high-chlorine iron oxide red and the permanent magnet prepared by the low-chlorine ferrite in the scheme of the invention have similar performance, which shows that the feasibility of the scheme is high; as can be seen from comparison of examples 1-3, the higher the chlorine content in the iron oxide red, the higher the final residual chlorine content, which in turn affects the permanent magnetic properties of the ferrite.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. A method for preparing permanent magnetic ferrite from high-chlorine iron oxide red is characterized by comprising the following steps:
a) iron oxide red pretreatment: according to the proportion of 1: 0.5-1.0: mixing and ball-milling iron oxide red containing 0.15-0.3% of chlorine element, a solvent and a dispersant in a mass ratio of 0.0005-0.002 to obtain uniform slurry;
b) dechlorination: spray drying the slurry obtained in the step a) at the temperature of 100 ℃ and 300 ℃ to obtain a main material;
c) preparation of Pre-fired raw Material SrO.MFe2O3: mixing the main material and the auxiliary material obtained in the step b) according to the proportion M of 5.2-6.5, then adding an additive A accounting for 0-6 wt% of the mixed material, adding ball milling liquid according to the mass ratio of 1:0.9-1.1, performing ball milling to obtain uniform powder, and then drying to obtain a pre-sintered raw material; the presintering raw material is SrO.MFe2O3The strontium ferrite mixture of (1);
d) pre-burning: sintering the pre-sintering raw material prepared in the step c) at 1200-;
e) and (3) secondary grinding: grinding and ball-milling the ferrite pre-sintered material to obtain coarse powder, adding an additive B with the mass fraction of 0-6 wt% into the coarse powder, and ball-milling again to obtain fine slurry;
f) and (3) sintering: and e) pressing and molding the fine slurry obtained in the step e), and sintering at the temperature of 1200-1300 ℃ for 1-3 hours to obtain the permanent magnetic ferrite.
2. The method of claim 1, wherein in the step a), the uniform slurry has a particle size of 1 to 1.5 μm; the solvent is deionized water; the dispersing agent is calcium stearate.
3. The method of claim 1, wherein the chlorine content of the main material in step b) is 0.001-0.01 wt%.
4. The method of claim 1, wherein in step c), the ingredient is strontium carbonate; the additive A is one or more of silicon dioxide, aluminum oxide or calcium carbonate or boric acid; the ball milling liquid is water; the particle size of the uniform powder is 0.5-1.0 μm.
5. The method of claim 1, wherein in step d), the pre-firing process is performed in air; the sintering condition of the pre-sintering raw material is 1260-1300 ℃, and the temperature is kept for 1-2 hours.
6. The method of claim 1, wherein in step e), the coarse powder has a particle size of 3.5 to 5 μm; the additive B is one or a mixture of more of calcium carbonate, strontium carbonate, silicon dioxide, aluminum oxide and boric acid; the grain diameter of the fine slurry is 0.6-1.0 μm.
7. The method of claim 1, wherein the press-molding in step f) is a wet press-molding method comprising the steps of:
1) standing and filtering the fine slurry obtained in the step e);
2) after water filtration, press forming is carried out, and simultaneously, a forming magnetic field of 9000-11000Oe is applied in the pressing direction.
8. The method according to claim 7, wherein in the step 2), the molding pressure is 3 to 5 MPa.
9. The method according to claim 1, wherein in step f), the sintering temperature is 1230-1260 ℃ and the holding time is 1.5-2.5 hours.
10. A permanent magnetic ferrite prepared by any one of the methods of claims 1 to 9.
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