CN103145409A - Manufacturing method of dry-type anisotropic strontium ferrite - Google Patents
Manufacturing method of dry-type anisotropic strontium ferrite Download PDFInfo
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- CN103145409A CN103145409A CN2013100771654A CN201310077165A CN103145409A CN 103145409 A CN103145409 A CN 103145409A CN 2013100771654 A CN2013100771654 A CN 2013100771654A CN 201310077165 A CN201310077165 A CN 201310077165A CN 103145409 A CN103145409 A CN 103145409A
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Abstract
The invention relates to a manufacturing method of dry-type anisotropic strontium ferrite, which uses Fe2O3 and SrCO3 as raw materials, CaCO3 and SiO2 as additives, and synthetic wax and calcium stearate respectively as a binding agent and a forming assistant. The manufacturing method comprises the following steps: preparing presintered fine powder, preparing a compound concentrated material, preparing fine powder for formation, and forming by sintering. The synthetic wax is used as the binding agent instead the traditional camphor binding agent, thereby reducing the hazards to life and environmental pollution due to use of camphor; and besides, the density of the sintered body can be enhanced to avoid generating bee-holes on the product surface, thereby forming the dry-type anisotropic strontium ferrite with excellent magnetic properties.
Description
Technical field
The present invention relates to ferritic manufacture method, be specifically related to a kind of manufacture method of dry type anisotropy strontium ferrites.
Background technology
In the production technique of traditional dry type anisotropy strontium ferrites, usually need to camphorate as tackiness agent.Its is easily volatilization and produce the gas of a large amount of irritating smells at normal temperatures, and human body is had certain harm, also can cause very large pollution to environment simultaneously.If the heavy dose of contact of industrial worker can cause the cardiomotility paralysis, cause serious spasm.To use camphor and calcium stearate as forming adhesive at present substantially in industrial production, although materials such as occurring use fatty acid series ester type waxes in a small amount of document and patent is also arranged, but because it belongs to natural phant wax, wherein contain the material that the part difficulty is decomposed, fusing point is high, after interpolation, a large amount of bee-holes occurs through sintered products surface meeting, their hardness is large simultaneously, viscosity and oilness do not reach well lubricated, dispersion effect yet, therefore are not suitable for industrial production.
Summary of the invention
The object of the present invention is to provide a kind of manufacture method of dry type anisotropy strontium ferrites, it uses synthetic wax as tackiness agent, can reduce because of use that camphor causes to the harm of the person with to the pollution of environment, can also improve sintered density, avoid product surface to produce bee-hole, form the dry type anisotropy strontium ferrites with superior magnetic property.
The technical solution adopted for the present invention to solve the technical problems is:
(1) preparation pre-burning fine powder material
Fe in molar ratio
2O
3: SrCO
3=5.7-5.9:1 takes raw material Fe
2O
3And SrCO
3, through mixing, oven dry, pre-burning, coarse breaking, obtain the meal material, then add the CaCO of the 0.8-1.25wt% of this meal material weight
3And the SiO of 0.08-0.3wt%
2, then, oven dry broken through fine powder, obtain the pre-burning fine powder material;
(2) prepare mixing concentrate feed
Take step (1) gained pre-burning fine powder material and mix with synthetic wax as tackiness agent, wherein synthetic wax accounts for 1-12wt%, and the pre-burning fine powder material accounts for 99-88wt%, drops into Banbury mixer after mixing, and is cooled to room temperature after adding hot milling, obtains mixing concentrate feed;
(3) preparation moulding fine powder
Take the mixing concentrate feed of step (2) gained and step (1) gained pre-burning fine powder material mixes with mass ratio 1:9, obtain the mixture that synthetic wax accounts for 0.1-1.2wt%, the moulding auxiliary calcium stearate that adds again the 0.05-1.2wt% of this mixture weight, through mixing, Crushing of Ultrafine, obtain the moulding fine powder;
(4) forming and sintering
Use fine powder through moulding, sintering, grinding step (3) gained moulding, obtain dry type anisotropy strontium ferrites of the present invention.
Described synthetic wax is the brown color blocks of solid, and molecular weight is that 200-600, carbonatoms are the hydrocarbon mixture of 4-26, and main component is straight-chain paraffin, also contains simultaneously naphthenic hydrocarbon, isoparaffin, aromatic hydrocarbon, unsaturated hydrocarbons or their mixture.
The density of described synthetic wax is 0.990-0.999g/cm
3, fusing point is 58-79 ℃, and is water insoluble, is dissolved in hot ethanol.
Preferably, in step (2), synthetic wax accounts for 1.5-8wt%.
More preferably, in step (2), synthetic wax accounts for 2-6wt%.
In step (1), the mean particle size of pre-burning fine powder material is 0.65-0.8 μ m, is preferably 0.7-0.75 μ m.
The time that adds hot milling in step (2) is 10-25min.
The synthetic wax tackiness agent that the present invention adds, it is a kind of brown color blocks of solid material, molecular weight is about the hydrocarbon mixture that 200-600, carbonatoms are about 4-26, and main component is straight-chain paraffin, also has simultaneously a small amount of naphthenic hydrocarbon, isoparaffin, aromatic hydrocarbon, unsaturated hydrocarbons or their mixture.Density is 0.990-0.999g/cm
3, fusing point is 58-79 ℃, and is water insoluble, is dissolved in the organic solvents such as hot ethanol, can help esterifying agent, slightly acidic esterifying catalyst, organic salt catalyzer etc. to make through techniques such as catalyzed oxidation, nitrogen esterifications by adding higher alcohols in the food-class high-purity Microcrystalline Wax.
Synthetic wax is as tackiness agent, and its addition in product (being content) is 0.1-1.2wt%.Addition is very few, can not bring into play effect, and particle and magnetocrystalline orientation degree are bad, the formability variation; Addition is too much, and organic carbonization in the time of can causing sintering and the density of sintered compact is descended makes Br equimagnetic degradation.
Also added the moulding auxiliary calcium stearate of 0.05-1.2wt% when adding the synthetic wax tackiness agent, addition is preferably 0.1-0.8wt%.Can effectively improve formability, improve mobility and the power of reducing friction by adding the moulding auxiliary, can further improve magnetic property.
The invention has the beneficial effects as follows:
Owing to replacing camphor as tackiness agent with synthetic wax in the manufacture method of dry type anisotropy strontium ferrites, have benefited from the characteristic of its difficult volatilization, so in reaction system, the addition of tackiness agent can not reduce along with the carrying out of whole technological process; Can reduce production costs, reduce to use camphor as tackiness agent cause to the harm of the person with to the pollution of environment; The heat decomposition temperature of synthetic wax is wider, slowly decompose in 100-500 ℃ of scope, final temperature of having decomposed is lower than the formation temperature of strontium ferrites, when it is in molten state, has good mobility, can penetrate into better in the powder gap, be conducive to the moulding of magnet and the raising of density, can also avoid green compact cracking and sintered compact surface bee-hole to occur; Synthetic wax also has good oilness simultaneously, then reduces the frictional force that in moulding process, ferrite particle rotates, and is conducive to improve the orientation degree of particle and magnetocrystalline.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
Adopt following steps to make product of the present invention:
(1) preparation pre-burning fine powder material
Fe in molar ratio
2O
3: SrCO
3=5.7:1 takes raw material Fe
2O
3And SrCO
3Mixing, oven dry and pre-burning obtain Preburning material.Use vibromill to become mean particle size to be the meal material of 2-6 μ m above-mentioned Preburning material coarse breaking, add the CaCO of the 0.8wt% of this meal material weight
3And the SiO of 0.3wt%
2After, fine powder is broken into the fine powder post-drying that mean particle size is 0.8 μ m, obtains the pre-burning fine powder material.
(2) prepare mixing concentrate feed
Take step (1) gained pre-burning fine powder material and mix with synthetic wax, wherein synthetic wax accounts for 1wt%, and the pre-burning fine powder material accounts for 99wt%, and mixed material is dropped into Banbury mixer, carries out mixing in the time of heating.When temperature rises to 75 ℃, open cooling water circulationly, control temperature 80 ℃ of left and right, mix 15min, mix being cooled to room temperature after completing, obtain mixing concentrate feed.
(3) preparation moulding fine powder
Take the mixing concentrate feed of step (2) gained and step (1) gained pre-burning fine powder material mixes with mass ratio 1:9, obtain the mixture that synthetic wax accounts for 0.1wt%, the moulding auxiliary calcium stearate that adds again the 0.8wt% of this mixture weight, use double worm mixer mixing 15min, then by mechanical dispersion equipment Crushing of Ultrafine, obtain the moulding fine powder.
(4) forming and sintering
Use 45T semi-automatic liquid press that step (3) gained moulding is molded into fine powder
Right cylinder, and carry out sintering, grinding, obtain dry type anisotropy strontium ferrites of the present invention.
Embodiment 2
Adopt following steps to make product 4 of the present invention:
(1) preparation pre-burning fine powder material
Fe in molar ratio
2O
3: SrCO
3=5.8:1 takes raw material Fe
2O
3And SrCO
3Mixing, oven dry and pre-burning obtain Preburning material.Use vibromill to become mean particle size to be the meal material of 2-6 μ m above-mentioned Preburning material coarse breaking, add the CaCO of the 1.1wt% of this meal material weight
3And the SiO of 0.2wt%
2After, fine powder is broken into the fine powder post-drying that mean particle size is 0.72 μ m, obtains the pre-burning fine powder material.
(2) prepare mixing concentrate feed
Take step (1) gained pre-burning fine powder material and mix with synthetic wax, wherein synthetic wax accounts for 6wt%, and the pre-burning fine powder material accounts for 94wt%, and mixed material is dropped into Banbury mixer, carries out mixing in the time of heating.When temperature rises to 75 ℃, open cooling water circulationly, control temperature 80 ℃ of left and right, mix 15min, mix being cooled to room temperature after completing, obtain mixing concentrate feed.
(3) preparation moulding fine powder
Take the mixing concentrate feed of step (2) gained and step (1) gained pre-burning fine powder material mixes with mass ratio 1:9, obtain the mixture that synthetic wax accounts for 0.6wt%, the moulding auxiliary calcium stearate that adds again the 0.4wt% of this mixture weight, use double worm mixer mixing 20min, then by mechanical dispersion equipment Crushing of Ultrafine, obtain the moulding fine powder.
(4) forming and sintering
Use 45T semi-automatic liquid press that step (3) gained moulding is molded into fine powder
Right cylinder, and carry out sintering, grinding, obtain dry type anisotropy strontium ferrites of the present invention.
Embodiment 3
Adopt following steps to make product of the present invention:
(1) preparation pre-burning fine powder material
Fe in molar ratio
2O
3: SrCO
3=5.9:1 takes raw material Fe
2O
3And SrCO
3Mixing, oven dry and pre-burning obtain Preburning material.Use vibromill to become mean particle size to be the meal material of 2-6 μ m above-mentioned Preburning material coarse breaking, add the CaCO of the 1.25wt% of this meal material weight
3And the SiO of 0.1wt%
2After, fine powder is broken into the fine powder post-drying that mean particle size is 0.65 μ m, obtains the pre-burning fine powder material.
(2) prepare mixing concentrate feed
Take step (1) gained pre-burning fine powder material and mix with synthetic wax, wherein synthetic wax accounts for 12wt%, and the pre-burning fine powder material accounts for 88wt%, and mixed material is dropped into Banbury mixer, carries out mixing in the time of heating.When temperature rises to 75 ℃, open cooling water circulationly, control temperature 80 ℃ of left and right, mix 25min, mix being cooled to room temperature after completing, obtain mixing concentrate feed.
(3) preparation moulding fine powder
Take the mixing concentrate feed of step (2) gained and step (1) gained pre-burning fine powder material mixes with mass ratio 1:9, obtain the mixture that synthetic wax accounts for 1.2wt%, the moulding auxiliary calcium stearate that adds again the 0.1wt% of this mixture weight, use double worm mixer mixing 25min, then by mechanical dispersion equipment Crushing of Ultrafine, obtain the moulding fine powder.
(4) forming and sintering
Use 45T semi-automatic liquid press that step (3) gained moulding is molded into fine powder
Right cylinder, and carry out sintering, grinding, obtain dry type anisotropy strontium ferrites of the present invention.
Embodiment 4
Adopt the method for embodiment 2, when wherein the pre-burning fine powder material mixes with synthetic wax in step (2), synthetic wax accounts for 2wt%, prepares product 1 of the present invention.
Embodiment 5
Adopt the method for embodiment 2, when wherein the pre-burning fine powder material mixes with synthetic wax in step (2), synthetic wax accounts for 3wt%, prepares product 2 of the present invention.
Embodiment 6
Adopt the method for embodiment 2, when wherein the pre-burning fine powder material mixes with synthetic wax in step (2), synthetic wax accounts for 4wt%, prepares product 3 of the present invention.
Embodiment 7
Adopt the method for embodiment 2, when wherein the pre-burning fine powder material mixes with synthetic wax in step (2), synthetic wax accounts for 8wt%, prepares product 5 of the present invention.
Below for replace the Comparative Examples of synthetic wax with camphor.
Comparative Examples 1
Adopt following steps to make comparative sample 1:
(1) preparation pre-burning fine powder material
Fe in molar ratio
2O
3: SrCO
3=5.8:1 takes raw material Fe
2O
3And SrCO
3Mixing, oven dry and pre-burning obtain Preburning material.Use vibromill to become mean particle size to be the meal material of 2-6 μ m above-mentioned Preburning material coarse breaking, add the CaCO of the 1.1wt% of this meal material weight
3And the SiO of 0.2wt%
2After, fine powder is broken into the fine powder post-drying that mean particle size is 0.72 μ m, obtains the pre-burning fine powder material.
(2) preparation concentrate feed
Take step (1) gained pre-burning fine powder material and mix with camphor, wherein camphor accounts for 4wt%, and the pre-burning fine powder material accounts for 96wt%, and mixed material is dropped into Crushing of Ultrafine in mechanical dispersion equipment, obtains concentrate feed.(because the physical property of camphor highly volatile does not need to heat banburying, its concentrate feed also can mix uniformly with the pre-burning fine powder material)
(3) preparation moulding fine powder
Take step (2) gained concentrate feed and step (1) gained pre-burning fine powder material mixes with mass ratio 1:9, obtain the mixture that camphor accounts for 0.4wt%, the moulding auxiliary calcium stearate that adds again the 0.4wt% of this mixture weight, use double worm mixer mixing 20min, then by mechanical dispersion equipment Crushing of Ultrafine, obtain the moulding fine powder.
(4) forming and sintering
Use 45T semi-automatic liquid press that step (3) gained moulding is molded into fine powder
Right cylinder, and carry out sintering, grinding, obtain comparative sample 1.
Comparative Examples 2
Adopt the method for Comparative Examples 1, wherein camphor accounts for 8wt% in step (2), prepares comparative sample 2.
Comparative Examples 3
Adopt the method for Comparative Examples 1, wherein camphor accounts for 12wt% in step (2), prepares comparative sample 3.
The performance test methods of above embodiment and Comparative Examples products obtained therefrom is:
A) density of product is tested with drainage.
B) aspect magnetic property, the remanent magnetism Br of product, magnetic strength coercivity H b, HCJ Hcj adopt the B-H tester test of Loudi, Hunan electronics institute, exportable J-H loop line, BH loop, demagnetizing curve etc.Testing method: use the plane grinding machine to polish in sample, guarantee that the upper and lower surfaces of cake are all smooth smooth, and upper and lower surface is parallel to each other, then use the B-H tester to test under the 1500KA/m magnetic field condition, the test environment temperature is 23 ℃ of left and right.The repeatability of test result is: Br, Hcb, Hcj be ± and 0.2%.
Adopt above-mentioned testing method to carrying out performance test with the synthetic wax (product 1-5 of the present invention) of the present invention's employing and the camphor (comparative sample 1-3) of prior art employing as the dry type anisotropy strontium ferrites product that tackiness agent prepares respectively, the results are shown in following table 1.
Table 1 synthetic wax and camphor are as the product performance test result of tackiness agent
By finding out in table, as tackiness agent, at its product 1-5 of the present invention that more preferably adds (0.2-0.8wt%) in scope, follow with the comparative sample 1-3 of camphor as tackiness agent and compare: both have close density with synthetic wax; Produce bee-hole with camphor as the comparative sample 2,3 of tackiness agent, and all do not produced bee-hole with synthetic wax as the product 1-5 of the present invention of tackiness agent; Aspect magnetic property, with synthetic wax as the remanent magnetism Br of the product 1-5 of the present invention of tackiness agent, magnetic strength coercivity H b, HCJ Hcj than comparative sample 1-3, can reach substantially equal or slightly high level.
Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.After the content of having read the present invention's instruction, those skilled in the art can do various conversion or modification to the present invention with any same or similar means, within these equivalent form of values fall into protection scope of the present invention equally.
Claims (7)
1. the manufacture method of a dry type anisotropy strontium ferrites is characterized in that comprising following steps:
(1) preparation pre-burning fine powder material
Fe in molar ratio
2O
3: SrCO
3=5.7-5.9:1 takes raw material Fe
2O
3And SrCO
3, through mixing, oven dry, pre-burning, coarse breaking, obtain the meal material, then add the CaCO of the 0.8-1.25wt% of this meal material weight
3And the SiO of 0.08-0.3wt%
2, then, oven dry broken through fine powder, obtain the pre-burning fine powder material;
(2) prepare mixing concentrate feed
Take step (1) gained pre-burning fine powder material and mix with synthetic wax, wherein synthetic wax accounts for 1-12wt%, and the pre-burning fine powder material accounts for 99-88wt%, drops into Banbury mixer after mixing, and is cooled to room temperature after adding hot milling, obtains mixing concentrate feed;
(3) preparation moulding fine powder
Take the mixing concentrate feed of step (2) gained and step (1) gained pre-burning fine powder material and mix with mass ratio 1:9, then add the calcium stearate of the 0.05-1.2wt% of this mixture weight, through mixing, Crushing of Ultrafine, obtain the moulding fine powder;
(4) forming and sintering
Use fine powder through moulding, sintering, grinding step (3) gained moulding, obtain dry type anisotropy strontium ferrites of the present invention.
2. method according to claim 1, it is characterized in that: described synthetic wax is the hydrocarbon mixture of molecular weight 200-600, carbonatoms 4-26, main component is straight-chain paraffin, also contains simultaneously naphthenic hydrocarbon, isoparaffin, aromatic hydrocarbon, unsaturated hydrocarbons or their mixture.
3. method according to claim 2, it is characterized in that: the density of described synthetic wax is 0.990-0.999g/cm
3, fusing point is 58-79 ℃, and is water insoluble, is dissolved in hot ethanol.
4. method according to claim 1 is characterized in that: in described step (2), synthetic wax accounts for 1.5-8wt%.
5. method according to claim 4 is characterized in that: in described step (2), synthetic wax accounts for 2-6wt%.
6. method according to claim 1 is characterized in that: in described step (1), the mean particle size of pre-burning fine powder material is 0.65-0.8 μ m.
7. method according to claim 1, it is characterized in that: the time that adds hot milling in described step (2) is 10-25min.
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| CN103145409B CN103145409B (en) | 2015-06-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110143821A (en) * | 2019-06-24 | 2019-08-20 | 海安南京大学高新技术研究院 | The production method that adhesive is used in the molding of dry-pressing opposite sex permanent-magnet ferrite |
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|---|---|---|---|---|
| CN1664964A (en) * | 2005-03-17 | 2005-09-07 | 华南理工大学 | Process for clinkering anisotropic permanent ferrite through polymer bonding and modeling |
| CN101205137A (en) * | 2007-01-18 | 2008-06-25 | 横店集团东磁股份有限公司 | Method for manufacturing sintered permanent magnetic ferrite formed by dry pressing |
| CN101870579A (en) * | 2010-06-10 | 2010-10-27 | 上海应用技术学院 | Permanently magnetic strontium ferrite material and preparation method thereof |
| CN101989479A (en) * | 2009-08-03 | 2011-03-23 | 广东江粉磁材股份有限公司 | Method for manufacturing sintered iron strontium oxide permanent magnetic material |
-
2013
- 2013-03-11 CN CN201310077165.4A patent/CN103145409B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664964A (en) * | 2005-03-17 | 2005-09-07 | 华南理工大学 | Process for clinkering anisotropic permanent ferrite through polymer bonding and modeling |
| CN101205137A (en) * | 2007-01-18 | 2008-06-25 | 横店集团东磁股份有限公司 | Method for manufacturing sintered permanent magnetic ferrite formed by dry pressing |
| CN101989479A (en) * | 2009-08-03 | 2011-03-23 | 广东江粉磁材股份有限公司 | Method for manufacturing sintered iron strontium oxide permanent magnetic material |
| CN101870579A (en) * | 2010-06-10 | 2010-10-27 | 上海应用技术学院 | Permanently magnetic strontium ferrite material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110143821A (en) * | 2019-06-24 | 2019-08-20 | 海安南京大学高新技术研究院 | The production method that adhesive is used in the molding of dry-pressing opposite sex permanent-magnet ferrite |
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Address after: 529000 Longwan Road, Guangdong, China, No. 8, No. Patentee after: Guangdong led Limited by Share Ltd Address before: 529000 Longwan Road, Guangdong, China, No. 8, No. Patentee before: JPMF Guangdong Co., Ltd. |
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Effective date of registration: 20200813 Address after: No. 359, Jinou Road, Jianghai District, Jiangmen City, Guangdong Province:282 Nanshan Road, Jianghai District, Jiangmen City; 126 Gaoxin West Road, Jianghai District, Jiangmen City) No. 359, Jinou Road, Jianghai District, Jiangmen City, Guangdong Province (place of business: No. 282, Nanshan Road, Jianghai District, Jiangmen City; No. 126, Gaoxin West Road, Jianghai District, Jiangmen City) Patentee after: Jiangmen Jiangyi magnetic material Co.,Ltd. Address before: 529000 No. 8, Longwan Road, Jiangmen, Guangdong Patentee before: Guangdong led Limited by Share Ltd. |
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