CN113510244B - Method and device for producing flaky metal pigment - Google Patents
Method and device for producing flaky metal pigment Download PDFInfo
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- CN113510244B CN113510244B CN202110468822.2A CN202110468822A CN113510244B CN 113510244 B CN113510244 B CN 113510244B CN 202110468822 A CN202110468822 A CN 202110468822A CN 113510244 B CN113510244 B CN 113510244B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method and a device for producing a flaky metal pigment, wherein the production method comprises the following two-step grinding process: s1 rough grinding process: a ball mill with a larger diameter is matched with a group of grinding balls with a larger diameter, and the metal pigment raw material is quickly flaked by a process system of changing the rotating speed; s2 fine grinding process: a ball mill with a smaller diameter is matched with a group of grinding balls with a smaller diameter, and the grinding balls are shaped and polished for 2 to 4 hours; the production method of the flaky metal pigment disclosed by the invention can effectively reduce the grinding time, save energy, reduce consumption, improve the production efficiency and reduce the production cost; meanwhile, the product is not easy to be crushed, the particle size distribution can be controlled in a smaller range, and the particle size of the product is uniform.
Description
Technical Field
The invention relates to the field of metal powder deep processing, in particular to a method and a device for producing flaky metal pigment.
Background
The flake metallic pigment is widely used for various functional coatings such as anticorrosive coatings, conductive coatings, electromagnetic shielding coatings and the like. At present, various flaky metal pigments are mostly produced by adopting a traditional one-step grinding method, namely, granular metal powder is ground into flakes by one device, one group of balls and one set of process parameters. The method has the advantages of simple equipment, short process flow and lower production cost, but the surface shape of the product, the surface flatness of the sheet-mounted metallic pigment, the coating state of the surface and the like have more defects, thereby affecting the quality of the product. In the traditional grinding process, if a group of larger grinding balls are selected, the grinding speed is high, the required granularity is easily achieved, but the particles are not completely flaked and crushed due to the large ball diameter, or the flaked particles are smashed to pass through holes, or the edges of the flaked metal pigment particles are smashed to form incomplete flaked particles; if a group of grinding balls with smaller ball diameter is selected, the flaking process is slow, and the thickness of the flakes is too large, so that the diameter-thickness ratio of the produced particles does not meet the requirements of the product. Due to the defects, the coating made of the flaky metallic pigment is not compact, the functionality (such as corrosion resistance, conductivity, wave absorption and the like) of the coating is influenced, the appearance of the coating is not fine, and the metallic luster of the coating is poor. Therefore, providing a method for producing a flake metallic pigment to overcome the above-mentioned drawbacks is a technical problem to be solved urgently in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method and a device for producing a flaky metal pigment, wherein the method can effectively reduce grinding time, save energy, reduce consumption, improve production efficiency, reduce production cost, prevent the product from being crushed too easily, control the particle size distribution in a smaller range and ensure the uniform particle size of the product.
The technical scheme adopted by the invention is as follows:
a production method of a flaky metallic pigment is characterized by comprising the following two-step grinding process:
s1 rough grinding process: a ball mill with a larger diameter is matched with a group of grinding balls with a larger diameter, and the metal pigment raw material is rapidly flaked by a process of changing the rotating speed;
the method for changing the rotating speed comprises the following steps: when the ball mill starts to work, the ball mill is divided into a clockwise acceleration rotation stage t1 and a clockwise deceleration stage t 2; a counterclockwise acceleration rotation phase t3 and a counterclockwise deceleration rotation phase t 4; t1-t4 is one rough grinding cycle;
in the stages t1 and t3, the instantaneous speed n, in rpm, and the average diameter r of the grinding balls, in mm, are converted by the following formula along with the cumulative t, in units of s, of the running time of the stage: n is 100 t/r; the value of t is an integer from 1 to 20 in sequence;
S2 fine grinding process: and (4) shaping and polishing the product obtained in the step S1 by using a ball mill with a smaller diameter and a group of grinding balls with a smaller diameter.
For example, in the S1 rough grinding process, when the average diameter of the grinding balls is 10mm, clockwise rotation is accelerated at stage t1, and the instantaneous rotation speeds are sequentially, that is, n is 100/10 to 10rpm for the 1 st second, n is 100x2/20 to 20rpm for the 2 nd second, and so on, and up to 20 seconds, n is 100x20/10 to 200 rpm; the ball mill then proceeds to t2 for deceleration, and in this case, although not specifically defined, the ball mill may be decelerated linearly or at a rate corresponding to t1, and when the ball mill is decelerated to 0, the ball mill is accelerated counterclockwise with reference to the process of t1, and t1 to t4 are sequentially circulated. The coarse grinding is carried out by using the forward rotation and the reverse rotation which are gradually circulated, the flaky metal particles of the coarse grinding are completely flaky, the particles are uniform, and the technical scheme can bring more excellent coarse grinding effect.
Further, in the production method of the flake metal pigment, the metal pigment raw material is prepared by the following steps:
s1 raw material selection: collecting waste metal, manually selecting, and selecting a single metal raw material: including but not limited to one or more of silver, copper, iron, nickel, zinc, aluminum; or the alloy raw materials: including but not limited to one or more of zinc-aluminum alloy, aluminum-silicon alloy, copper-zinc alloy;
S2 pretreatment of raw materials: putting the metal raw materials into a pretreatment solution, soaking at 80-120 ℃ for 40-60 min, taking out, cleaning and drying;
s3 smelting: adopting a vacuum induction melting furnace, and solidifying into metal blocks after melting and purifying according to different melting points of various metals;
s4 crushing: placing the metal blocks into a metal crusher for primary crushing to obtain a metal pigment raw material with the average diameter of 3 mm;
the pretreatment solution comprises the following components in parts by weight:
further, in the coarse grinding process, 1-6 m is selected for coarse grinding3The vertical stirring ball mill or the horizontal roller ball mill; the diameter of a grinding ball selected for coarse grinding is 5-12 mm, the grinding ball can be a ball with a single diameter, or a plurality of balls with different diameters can be used in a compounding manner, and the material of the ball comprises but is not limited to steel, stainless steel or zirconia; the grinding temperature is 20-60 ℃, and the grinding time is 4-5 hours.
Further, in the production method of the flaky metal pigment, in the fine grinding process, 1-4 m is selected for fine grinding3The horizontal roller ball mill; the diameter of a grinding ball for fine grinding is 1-3 mm, the grinding ball can be a ball with a single diameter, or a plurality of balls with different diameters can be used in a compounding way, and the material of the ball comprises but is not limited to steel, stainless steel or zirconia; the grinding temperature is 20-60 ℃, and the grinding time is 2-4 hours.
Further, in the above method for producing a flake metallic pigment, both the coarse and fine milling may be dry milling or wet milling, the dry milling produces a powdery flake metallic pigment, and the wet milling produces a flake metallic pigment slurry.
Further, in the production method of the flaky metal pigment, the flaky metal pigment finely ground by the dry method is separated into the required granularity specification by an airflow classifier, or coarse powder exceeding the specification range of the product is screened out by a rotary vibrating screen, and then the flaky metal pigment powder can be obtained. In particular, the out of product specification range refers to a meal greater than 45 μm.
Further, in the production method of the flaky metal pigment, the flaky metal pigment finely ground by a wet method is subjected to separation by a cyclone classifier to obtain a required particle size specification, or coarse powder exceeding the product specification range is screened out by a rotary vibration sieve; most of the solvent can be removed from the graded flaky metal pigment slurry through filter pressing, the obtained filter cake is dispersed through a kneader, and a proper amount of auxiliary agent is added to obtain the flaky metal pigment paste. In particular, the specification of the granularity required by separation refers to the specification of products D50 such as 9 μm, 13 μm, 15 μm, 18 μm, 20 μm and the like respectively; the proper amount of the auxiliary agent refers to a compound auxiliary agent mainly comprising a plurality of dispersing agents.
Further, in the production method of the flaky metallic pigment, slurry obtained by wet coarse grinding can be directly subjected to pressure filtration, the obtained filter cake is subjected to vacuum drying to obtain powder, and then the powder is subjected to dry fine grinding and air classification or screening to obtain flaky metallic pigment powder.
Further, in the process of producing the powdery flaky metal pigment by dry grinding, a negative pressure unloading and conveying mode is adopted, a high-pressure centrifugal fan or a Rotz fan is used for sucking materials out of the ball mill, the materials are collected in a powder collecting bin through a cyclone dust collector or a bag dust collector, and then the materials are quantitatively and hermetically conveyed to a feeding port of an air classifier or a vibrating screen through a spiral feeder below the powder collecting bin, so that no dust leaks in the whole process.
Further, a production apparatus used in the above-mentioned production method of a flake metal pigment, said apparatus comprising a rough mill, a fine mill, a fan, a hopper, a screw feeder, and an air classifier or a vibrating screen feed port; the coarse grinding machine and the fine grinding machine are respectively connected with the fan, the fan is connected with the stock bin, and the stock bin is connected with the screw feeder; the spiral feeder is connected with a feed inlet of the airflow classifier or the vibrating screen; the whole process of grinding, conveying and airflow grading adopts inert gas protection.
Compared with the prior art, the invention has the following beneficial effects:
1. the method can effectively reduce the grinding time, save energy, reduce consumption, improve the production efficiency and reduce the production cost; compared with a one-stage mill, the power of 55KW takes 18h, the two-stage mill of the method uses 4h for coarse grinding of 55KW and 2h for fine grinding of 35KW, and the total time is 6h, so that 12h can be saved;
2. the product prepared by the method is not easy to be crushed, the particle size distribution can be controlled in a smaller range, and the particle size of the product is uniform;
3. the product prepared by the method has complete sheet shape, compact coating, excellent shielding property of the coating, strong corrosion resistance and metallic luster.
4. The method uses the recycled waste metal materials as raw materials for preparation, is green and environment-friendly, and changes waste into valuable.
Drawings
FIG. 1 is a schematic flow chart of the production process of the present invention;
FIG. 2 is an electron microscope image of the morphology of a product obtained by a single stage of the milling process of the present invention;
FIG. 3 is an electron microscope image of the morphology of the product obtained by the two-stage grinding process of the present invention;
FIG. 4 is a schematic view of a rough grinding machine and its associated equipment in the apparatus of the present invention;
FIG. 5 is a schematic view of a fine grinding machine and its associated apparatus in the apparatus of the present invention.
Detailed Description
Reference will now be made in detail to the embodiments of the present invention, examples of which are illustrated in the accompanying drawings, and which are intended to be illustrative of the invention and not to be construed as limiting the invention.
Examples
As shown in figures 1-5
A method for producing a flaky metallic pigment, comprising a two-step milling process of:
s1 rough grinding process: a ball mill with a larger diameter is matched with a group of grinding balls with a larger diameter, and the metal pigment raw material is rapidly flaked by a process of changing the rotating speed;
the method for changing the rotating speed comprises the following steps: when the ball mill starts to work, the ball mill is divided into a clockwise acceleration rotation stage t1 and a clockwise deceleration stage t 2; a counterclockwise acceleration rotation phase t3 and a counterclockwise deceleration rotation phase t 4; t1-t4 is one rough grinding cycle;
in the stages t1 and t3, the instantaneous speed n, in rpm, and the average diameter r of the grinding balls, in mm, are converted by the following formula along with the cumulative t, in units of s, of the running time of the stage: n is 100 t/r; the value of t is an integer from 1 to 20 in sequence;
s2 fine grinding process: a ball mill with a smaller diameter is matched with a group of grinding balls with a smaller diameter to shape and polish the product obtained in the step S1;
s1 raw material selection: collecting waste metal, manually selecting, and selecting a single metal raw material: including but not limited to one or more of silver, copper, iron, nickel, zinc, aluminum; or the alloy raw materials: including but not limited to one or more of zinc-aluminum alloy, aluminum-silicon alloy, copper-zinc alloy;
S2 pretreatment of raw materials: putting the metal raw materials into a pretreatment solution, soaking at 100 ℃ for 50min, taking out, cleaning and drying;
s3 smelting: adopting a vacuum induction melting furnace, and solidifying into metal blocks after melting and purifying according to different melting points of various metals;
s4 crushing: placing the metal blocks into a metal crusher for primary crushing to obtain a metal pigment raw material with the average diameter of 3 mm;
the pretreatment solution comprises the following components in parts by weight:
further, in the coarse grinding process, 1-6m is selected for coarse grinding3Preferably 3m, in a vertical stirred ball mill3；
Further, in the coarse grinding process, 1-6m is selected for coarse grinding3The horizontal roller ball mill; preferably 3m3；
Furthermore, the grinding balls for rough grinding have the diameter of 5-12 mm, can be balls with a single diameter, and can also be balls with different diameters for combined use, and the materials of the balls include but are not limited to steel, stainless steel or zirconia; the grinding temperature is 20-60 ℃, and the grinding time is 4-5 hours; preferably, the zirconia balls with the grinding balls with the diameter of 8mm are selected for coarse grinding; further preferably, zirconia balls with the diameters of 5 mm, 8mm and 12mm are selected for coarse grinding and compounded according to the proportion of 10:5: 1; the preferred grinding temperature is 45 ℃ and the grinding time is 4.5 hours;
Further, in the fine grinding process, 1-4 m is selected for fine grinding3The horizontal drum ball mill; preferably 2m3(ii) a The diameter of a grinding ball for fine grinding is 1-3 mm, the grinding ball can be a ball with a single diameter, or balls with different diameters can be compounded for use, and the material of the ball comprises but is not limited to steel, stainless steel or zirconia; the grinding temperature is 20-60 ℃, and the grinding time is 2-4 hours;
preferably, the fine grinding is performed by using stainless steel balls with the grinding ball diameter of 2 mm; further preferably, zirconia balls with the diameters of 1, 2 and 3mm are compounded according to the quantity ratio of 3:2:1 by fine grinding; the preferred grinding temperature is 40 ℃ and the grinding time is 3 hours;
further, both coarse and fine milling can be dry milling or wet milling, wherein the dry milling produces powdery flake metal pigment, and the wet milling produces slurry of the flake metal pigment;
further, the flaky metal pigment finely ground by the dry method is subjected to separation of required granularity specification by an airflow classifier, or coarse powder exceeding the specification range of the product is sieved by a rotary vibrating screen, and then the flaky metal pigment powder can be obtained; in particular, the out of product specification range refers to a meal greater than 45 μm;
further, the flake metal pigment finely ground by the wet method is required to be separated out of the required particle size specification by a cyclone classifier, or coarse powder exceeding the product specification range is screened out by a rotary vibration sieve; most of the solvent can be removed from the graded flaky metal pigment slurry through filter pressing, the obtained filter cake is dispersed through a kneader, and a proper amount of auxiliary agent is added to obtain flaky metal pigment paste; in particular, the specification of the granularity required by separation refers to the specification of products D50 such as 9 μm, 13 μm, 15 μm, 18 μm, 20 μm and the like respectively; the proper amount of the auxiliary agent refers to a compound auxiliary agent mainly comprising a plurality of dispersants;
Further, directly filter-pressing the slurry obtained by wet coarse grinding, drying the obtained filter cake into powder in vacuum, and then carrying out dry fine grinding and air flow classification or screening to obtain flaky metal pigment powder;
further, the slurry obtained by wet coarse grinding is directly subjected to pressure filtration, in the process of producing the powdery flaky metal pigment by dry grinding, a negative pressure unloading and conveying mode is adopted, a high-pressure centrifugal fan or a Rotz fan is used for sucking materials out of the ball mill, the materials are collected in a powder collecting bin through a cyclone dust collector or a bag dust collector, then the materials are quantitatively and hermetically conveyed to a feeding port of an air classifier or a vibrating screen through a spiral feeder below the powder collecting bin, and no dust leaks in the whole process;
further, the device comprises a coarse grinding machine, a fine grinding machine, a fan, a storage bin, a screw feeder and an air classifier or a vibrating screen feeding port; the coarse grinding machine and the fine grinding machine are respectively connected with the fan, the fan is connected with the stock bin, and the stock bin is connected with the screw feeder; the spiral feeder is connected with a feed inlet of the airflow classifier or the vibrating screen; the whole process of grinding, conveying and airflow grading adopts inert gas protection.
Performance testing
The particle size distribution results of the products obtained by different grinding processes using the same raw materials are compared, as shown in table 1; the raw materials are zinc-aluminum alloy, the first-stage grinding process is coarse grinding, and zirconia balls with the diameters of 5 mm, 8 mm and 12mm are selected and compounded according to the proportion of 10:5: 1; the grinding temperature is 45 ℃, and the grinding time is 4.5 hours; the two-stage grinding process comprises the steps of selecting zirconia balls with diameters of 1 mm, 2mm and 3mm respectively, and compounding according to the proportion of 3:2: 1; the grinding temperature is 40 ℃, and the grinding time is 3 hours; the remaining parameters were selected from the preferred parameters of the above examples.
Table 1 comparison of the particle size distribution results of the products obtained with the same raw materials and different milling processes:
as can be seen from the comparison of Table 1 and FIGS. 2 and 3, the product produced by the method of the present invention is not easily crushed, the particle size distribution can be controlled within a small range, and the particle size of the product is uniform.
The above are only preferred embodiments of the present invention, and the scope of the present invention should not be limited thereby, and all the equivalent changes and modifications made by the claims and the summary of the invention should be covered by the protection scope of the present patent application.
Claims (8)
1. A production method of a flaky metallic pigment is characterized by comprising the following two-step grinding process:
S1 rough grinding process: a ball mill with a larger diameter is matched with a group of grinding balls with a larger diameter, and the metal pigment raw material is rapidly flaked by a process of changing the rotating speed;
the method for changing the rotating speed comprises the following steps: when the ball mill starts to work, the ball mill is divided into a clockwise acceleration rotation stage t1 and a clockwise deceleration stage t 2; a counterclockwise acceleration rotation phase t3 and a counterclockwise deceleration rotation phase t 4; t1-t4 is one rough grinding cycle;
in the stages t1 and t3, the conversion between the instantaneous speed n, in rpm, and the average diameter r of the grinding balls, in mm, and the cumulative t, in s, of the running time of the stage is as follows: n is 100 t/r; the value of t is an integer from 1 to 20 in sequence;
s2 fine grinding process: a ball mill with a smaller diameter is matched with a group of grinding balls with a smaller diameter to shape and polish the product obtained in the step S1;
the metal pigment raw material is prepared by the following steps:
s1, selecting raw materials: collecting waste metal, manually selecting, and selecting a single metal raw material: including but not limited to one of silver, copper, iron, nickel, zinc, aluminum; or the alloy raw materials: including but not limited to one or more of zinc-aluminum alloy, aluminum-silicon alloy, copper-zinc alloy;
s2 raw material pretreatment: putting the metal raw materials into a pretreatment solution, soaking at 80-120 ℃ for 40-60 min, taking out, cleaning and drying;
S3 smelting: adopting a vacuum induction melting furnace, and solidifying into metal blocks after melting and purifying according to different melting points of various metals;
s4 crushing: placing the metal blocks into a metal crusher for primary crushing to obtain a metal pigment raw material with the average diameter of 3 mm;
the pretreatment solution consists of the following components in parts by weight:
2. the method for producing a flaky metallic pigment according to claim 1, wherein in the coarse grinding process, 1-6 m is selected for coarse grinding3The vertical stirring ball mill or the horizontal roller ball mill; the diameter of a grinding ball for coarse grinding is 5-12 mm, the grinding ball can be a ball with a single diameter, or balls with different diameters can be used in a compounding mode, and the ball is made of one of steel, stainless steel or zirconia; the grinding temperature is 20-60 ℃, and the grinding time is 4-5 hours.
3. The method for producing a flaky metallic pigment according to claim 1, wherein in the fine grinding process, 1 to 4m is selected for fine grinding3The horizontal roller ball mill; the diameter of a grinding ball for fine grinding is 1-3 mm, the grinding ball can be a ball with a single diameter, or balls with different diameters can be compounded for use, and the material of the ball comprises but is not limited to one of steel, stainless steel or zirconia; the grinding temperature is 20-60 ℃, and the grinding time is 2-4 hours.
4. The process for producing a flaky metallic pigment according to claim 1, wherein both the coarse and fine milling are carried out by dry milling to produce a flaky metallic pigment in the form of powder or wet milling to produce a slurry of the flaky metallic pigment.
5. The process for producing a flaky metallic pigment according to claim 4, wherein the flaky metallic pigment finely ground by the dry process is subjected to classifying by an air classifier to obtain a desired particle size specification or sieving by a rotary vibrating sieve to obtain a coarse powder exceeding the specification range of the product, thereby obtaining a flaky metallic pigment powder.
6. The process for producing a flaky metallic pigment according to claim 4, wherein the flaky metallic pigment finely ground by the wet process is subjected to classifying by a cyclone classifier to obtain a desired particle size specification or sieving by a rotary vibrating sieve to obtain coarse powder outside the specification range of the product; most of the solvent can be removed from the graded flaky metal pigment slurry through filter pressing, the obtained filter cake is dispersed through a kneader, and a proper amount of auxiliary agent is added to obtain the flaky metal pigment paste.
7. The process for producing a flaky metallic pigment according to claim 4, wherein the slurry obtained by wet coarse grinding is subjected to pressure filtration directly, the obtained filter cake is vacuum-dried to a powdery form, and then subjected to dry fine grinding, air classification or screening to obtain a flaky metallic pigment powder.
8. The method according to claim 4, wherein during the dry milling process, the powder of flake metal pigment is discharged and conveyed under negative pressure by a high pressure centrifugal fan or a Roots blower, and the material is collected in a dust collecting bin by a cyclone or a bag collector and then quantitatively and hermetically conveyed to the feed inlet of the air classifier or the vibrating screen by a screw feeder below the dust collecting bin without dust leakage in the whole process.
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