CN116313359B - Production process of manganese zinc ferrite slurry with high solid content - Google Patents
Production process of manganese zinc ferrite slurry with high solid content Download PDFInfo
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- CN116313359B CN116313359B CN202310156661.2A CN202310156661A CN116313359B CN 116313359 B CN116313359 B CN 116313359B CN 202310156661 A CN202310156661 A CN 202310156661A CN 116313359 B CN116313359 B CN 116313359B
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- 239000002002 slurry Substances 0.000 title claims abstract description 90
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 title claims abstract description 67
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
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- 238000002156 mixing Methods 0.000 claims abstract description 85
- 238000000498 ball milling Methods 0.000 claims abstract description 72
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- 239000002904 solvent Substances 0.000 claims abstract description 65
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- 239000002131 composite material Substances 0.000 claims abstract description 40
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002270 dispersing agent Substances 0.000 claims abstract description 33
- 239000011230 binding agent Substances 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000007822 coupling agent Substances 0.000 claims abstract description 21
- 239000012188 paraffin wax Substances 0.000 claims abstract description 19
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 17
- 239000004200 microcrystalline wax Substances 0.000 claims abstract description 17
- 235000019808 microcrystalline wax Nutrition 0.000 claims abstract description 17
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008117 stearic acid Substances 0.000 claims abstract description 17
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000001993 wax Substances 0.000 claims abstract description 13
- 239000011701 zinc Substances 0.000 claims abstract description 10
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 235000019809 paraffin wax Nutrition 0.000 claims abstract description 3
- 235000019271 petrolatum Nutrition 0.000 claims abstract description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 46
- 239000000463 material Substances 0.000 claims description 36
- 229910000831 Steel Inorganic materials 0.000 claims description 24
- 239000010959 steel Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 17
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 15
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 15
- 229960004494 calcium gluconate Drugs 0.000 claims description 15
- 239000004227 calcium gluconate Substances 0.000 claims description 15
- 235000013927 calcium gluconate Nutrition 0.000 claims description 15
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims description 15
- 239000000600 sorbitol Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 238000009849 vacuum degassing Methods 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 15
- 239000002245 particle Substances 0.000 description 14
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 11
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 11
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 11
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 11
- 239000005642 Oleic acid Substances 0.000 description 11
- 239000004721 Polyphenylene oxide Substances 0.000 description 11
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 11
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 11
- 229920000570 polyether Polymers 0.000 description 11
- 229920002545 silicone oil Polymers 0.000 description 11
- 239000000696 magnetic material Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 238000011161 development Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
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- 235000013871 bee wax Nutrition 0.000 description 1
- 239000012166 beeswax Substances 0.000 description 1
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- 239000006185 dispersion Substances 0.000 description 1
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- 239000008187 granular material Substances 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- 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
- H01F1/12—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 soft-magnetic materials
- H01F1/34—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 soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Magnetic Ceramics (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention relates to the technical field of ferrite production processes, and discloses a production process of manganese zinc ferrite slurry with high solid content. The production process of the high-solid-content manganese zinc ferrite slurry comprises the following steps of: taking a mixture of a composite dispersing agent, manganese zinc ferrite powder and a solvent for proportioning; adding the mixture into a ball mill for ball milling and mixing to obtain a grinding product A; adding the mixture into a high-energy ball mill for ball milling and mixing to obtain a grinding product B; heating paraffin wax, microcrystalline wax, stearic acid and dibutyl phthalate to obtain soluble composite wax, and adding a coupling agent to obtain a soluble binder; taking a grinding product A, a grinding product B, a dispersing agent, a soluble binder, a defoaming agent and a solvent to obtain slurry; and filtering and vacuum defoaming the slurry to obtain the high-solid-content Mn-Zn ferrite slurry. The manganese zinc ferrite slurry obtained by the method has high solid content and good fluidity, and can effectively reduce the production cost.
Description
Technical Field
The invention relates to the technical field of ferrite production processes, in particular to a production process of manganese zinc ferrite slurry with high solid content.
Background
The magnetic material plays an important role in information storage, processing and transmission, is widely applied to the fields of telecommunication, automatic control, communication, household appliances and the like, and the yield and the use amount of the magnetic material become one of marks for measuring the development degree of national economy and information technology. Soft magnetic materials are important functional materials, and have been widely used in aerospace, communication, automatic control, computer technology, broadcast television, etc. With the rapid development of the electronic information industry, the demand of high-performance soft magnetic materials is greatly increased, and each large magnetic material production company is invested in huge research, development and production of the high-performance soft magnetic materials, so that a good development opportunity is brought to the soft magnetic materials.
The soft magnetic material has the greatest dosage and the widest application range, and the soft magnetic ferrite material is mainly manganese zinc ferrite in the production and the use of the soft magnetic ferrite. The Mn-Zn ferrite material is one basic magnetic material for electronic industry and electromechanical industry with wide application, high yield and low cost, and its application directly affects the development of electronic technology, household appliance industry, computer and communication, environment protection and energy saving technology.
In the process of manufacturing the manganese zinc ferrite, the preparation of the particles is a key process, which determines the final quality level of the product. The slurry production is the basis for ensuring the quality of the granular materials, and the preparation of the manganese zinc ferrite slurry with high solid content and good fluidity has very important practical significance.
Disclosure of Invention
In order to solve the technical problems, the invention provides a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
and (3) proportioning: mixing a mixture of a composite dispersing agent, manganese zinc ferrite powder and a solvent, wherein the composite dispersing agent comprises calcium gluconate, triethanolamine and sorbitol;
In the process, the composite dispersing agent increases the repulsive energy of the surface of the manganese zinc ferrite powder by electrostatic action and steric hindrance, so that powder particles are promoted to be stably suspended in a medium.
Step (2), adding the mixture obtained in the step (1) into a ball mill to perform ball milling and mixing to obtain a grinding product A;
Step (3), adding the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B;
step (4) taking paraffin, microcrystalline wax, stearic acid and dibutyl phthalate, heating and mixing until uniformity is achieved, obtaining soluble composite wax, adding a coupling agent, stirring uniformly, cooling to room temperature, and crushing to obtain a soluble binder;
Step (5) taking the grinding product A, the grinding product B, a dispersing agent, a soluble binder, a defoaming agent and a solvent, and stirring and mixing to obtain slurry;
and (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming to obtain the manganese zinc ferrite slurry with high solid content.
Preferably, in the step (1), the ratio of each component in the mixture is: 0.5-2% of composite dispersant, 66-79% of manganese zinc ferrite powder and the balance of solvent; the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1; the mass ratio of the calcium gluconate to the triethanolamine to the sorbitol in the composite dispersing agent is 1:1:1.
Preferably, in the step (2), the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:400-600, the ball milling rotating speed is 60-240r/min, the ball milling time is 60-180min, the ball-material ratio is 4-6:1, and the granularity D50 of the ground product A is 1.2-1.8 mu m.
Preferably, in the step (3), the ball milling rotating speed is 800-1200r/min, the ball-material ratio is 4-6:1, the ball milling time is 80-120min, and the granularity D50 of the ground product B is 150-250nm.
Preferably, in the step (4), the mass ratio of paraffin wax, microcrystalline wax, stearic acid and dibutyl phthalate is 4.73:1.18:1.5:0.97, and the heating temperature is 60-80 ℃.
Preferably, in the step (4), the coupling agent is a coupling agent KH560, and the mass ratio of the coupling agent to the paraffin wax is 4.73:0.26-1.06.
Preferably, in the step (5), the ratio of each component in the slurry is: 42-50% of grinding product A, 20-28% of grinding product B, 0.25-0.5% of dispersing agent, 3.5-11% of soluble binder, 0.1-1% of defoaming agent and the balance of solvent.
Preferably, in the step (5), the slurry mixing time is 3-10 hours, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Preferably, in the step (6), the vacuum defoaming time is 30-60min.
Preferably, the high-solid content manganese zinc ferrite slurry prepared by adopting the production process of the high-solid content manganese zinc ferrite slurry.
Compared with the prior art, the invention has the beneficial effects that:
1. In the production process of the high-solid-content manganese zinc ferrite slurry, the composite dispersing agent formed by mixing calcium gluconate, triethanolamine, sorbitol and the like in a mass ratio is adopted, so that the dispersibility of the manganese zinc ferrite can be effectively improved, the water consumption is reduced, the solid content is improved, the slurry viscosity is reduced, the mobility of the slurry is increased, the power consumption in the production process is reduced, and the production cost is reduced.
2. In the mixing process of the soluble binder and the Mn-Zn ferrite, the Mn-Zn ferrite and the soluble compound wax (paraffin and microcrystalline wax) are connected through the coupling agent, so that on one hand, the dispersion of the Mn-Zn ferrite in the solvent is promoted, and on the other hand, the fluidity of a slurry system can be further improved due to the lubrication effect of the soluble compound paraffin.
3. According to the production process of the high-solid-content manganese zinc ferrite slurry, two grinding modes are adopted, a large-particle-size grinding product A obtained by ball milling of a ball mill is mixed with a small-particle-size grinding product B obtained by a high-energy ball mill, the small-particle-size grinding product B in the slurry can be distributed in particle gaps of the large-particle-size grinding product A, and the space utilization rate can be improved by mixing and arrangement of large particles and small particles, so that the solid content of emulsion is improved; in addition, the granularity of the grinding product B is nano-scale, and the nano-particles can be connected with a coupling agent, so that the agglomeration of the nano-particles is reduced.
Drawings
FIG. 1 is a flow chart of a process for preparing a high solids manganese zinc ferrite slurry of the present invention;
FIG. 2 is a plot of slurry concentration test comparisons for the high solids manganese zinc ferrite slurries of examples 1-5 and comparative examples 1-5 of the present invention;
FIG. 3 is a graph comparing slurry viscosity tests for high solids manganese zinc ferrite slurries of examples 1-5 and comparative examples 1-5 in accordance with the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
Example 1
The embodiment discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
The method comprises the following steps of (1) taking 100kg of a mixture of a composite dispersing agent, manganese zinc ferrite powder and a solvent, wherein the mixture comprises 0.5kg of the composite dispersing agent, 66kg of the manganese zinc ferrite powder and the balance of the solvent, the composite dispersing agent is obtained by mixing calcium gluconate, triethanolamine and sorbitol according to a mass ratio of 1:1:1, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), 60kg of the mixture obtained in the step (1) is added into a ball mill to perform ball milling and mixing, so as to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:400, the ball milling rotating speed is 60r/min, the ball milling time is 60min, the ball-material ratio is 4:1, and the granularity D50 of the grinding product A is 1.8 mu m.
Step (3), adding 40kg of the mixture obtained in the step (1) into a high-energy ball mill for ball milling and mixing to obtain a grinding product B; ball milling speed is 800r/min, ball material ratio is 4:1, ball milling time is 80min, and particle size D50 of ground product B is 250nm.
Step (4) taking 4.73kg of paraffin wax, 1.18kg of microcrystalline wax, 1.5kg of stearic acid and 0.97kg of dibutyl phthalate, uniformly mixing at 60 ℃ to obtain soluble composite wax, adding 0.26kg of coupling agent KH560, uniformly stirring, cooling to room temperature, and crushing to obtain the soluble binder.
Step (5) taking 42kg of grinding product A, 20kg of grinding product B, 0.25kg of oleic acid, 3.5kg of soluble binder, 0.1kg of polyether modified silicone oil and the balance of solvent, stirring and mixing the materials for 3 hours to obtain slurry, wherein the total weight of the materials is 100 kg; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming for 30min to obtain the high-solid-content manganese zinc ferrite slurry.
Example 2
The embodiment discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
taking 100kg of a mixture of a composite dispersing agent, 2kg of manganese zinc ferrite powder and 79kg of a solvent, wherein the mixture comprises the composite dispersing agent, the manganese zinc ferrite powder and the solvent, the composite dispersing agent is obtained by mixing calcium gluconate, triethanolamine and sorbitol according to a mass ratio of 1:1:1, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), 80kg of the mixture obtained in the step (1) is added into a ball mill to perform ball milling and mixing, so as to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:600, the ball milling rotating speed is 240r/min, the ball milling time is 180min, the ball-material ratio is 6:1, and the granularity D50 of the grinding product A is 1.2 mu m.
Step (3), adding 20kg of the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B; ball milling speed is 1200r/min, ball material ratio is 6:1, ball milling time is 120min, and particle size D50 of ground product B is 150nm.
Step (4) taking 4.73kg of paraffin wax, 1.18kg of microcrystalline wax, 1.5kg of stearic acid and 0.97kg of dibutyl phthalate, uniformly mixing at 80 ℃ to obtain soluble composite wax, adding 1.06kg of coupling agent KH560, uniformly stirring, cooling to room temperature, and crushing to obtain the soluble binder.
Step (5) taking 50kg of grinding product A, 28kg of grinding product B, 0.5kg of oleic acid, 11kg of soluble binder, 1kg of polyether modified silicone oil and the balance of solvent, and stirring and mixing the materials for 10 hours to obtain slurry; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming for 60min to obtain the high-solid-content manganese zinc ferrite slurry.
Example 3
The embodiment discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
Taking 100kg of a mixture of a composite dispersing agent, 1.3kg of manganese zinc ferrite powder and 71kg of a solvent, wherein the composite dispersing agent is obtained by mixing calcium gluconate, triethanolamine and sorbitol according to a mass ratio of 1:1:1, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), 70kg of the mixture obtained in the step (1) is added into a ball mill to perform ball milling and mixing, so as to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:500, the ball milling rotating speed is 140r/min, the ball milling time is 110min, the ball-material ratio is 5:1, and the granularity D50 of the grinding product A is 1.5 mu m.
Step (3), adding 30kg of the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B; ball milling speed is 1000r/min, ball material ratio is 5:1, ball milling time is 100min, and particle size D50 of ground product B is 200nm.
And (4) taking 4.73kg of paraffin wax, 1.18kg of microcrystalline wax, 1.5kg of stearic acid and 0.97kg of dibutyl phthalate, uniformly mixing at 70 ℃ to obtain soluble composite wax, adding 0.66kg of coupling agent KH560, uniformly stirring, cooling to room temperature, and crushing to obtain the soluble binder.
Step (5) taking 46kg of grinding product A, 24kg of grinding product B, 0.35kg of oleic acid, 7kg of soluble binder, 0.5kg of polyether modified silicone oil and the balance of solvent, and stirring and mixing the materials for 5 hours to obtain slurry, wherein the total weight of the solvent is 100 kg; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming for 40min to obtain the high-solid-content manganese zinc ferrite slurry.
Example 4
The embodiment discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
Taking 100kg of a mixture of 0.9kg of a composite dispersing agent, 68kg of manganese zinc ferrite powder and the balance of a solvent, wherein the composite dispersing agent is obtained by mixing calcium gluconate, triethanolamine and sorbitol according to a mass ratio of 1:1:1, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), adding 65kg of the mixture obtained in the step (1) into a ball mill to perform ball milling and mixing to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:450, the ball milling rotating speed is 100r/min, the ball milling time is 80min, the ball-material ratio is 4.5:1, and the granularity D50 of the grinding product A is 1.6 mu m.
Step (3), adding 35kg of the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B; ball milling speed is 900r/min, ball material ratio is 4.5:1, ball milling time is 90min, and particle size D50 of ground product B is 220nm.
Step (4) taking 4.73kg of paraffin wax, 1.18kg of microcrystalline wax, 1.5kg of stearic acid and 0.97kg of dibutyl phthalate, uniformly mixing at 65 ℃ to obtain soluble composite wax, adding 0.46kg of coupling agent KH560, uniformly stirring, cooling to room temperature, and crushing to obtain the soluble binder.
Step (5) taking 44kg of grinding product A, 22kg of grinding product B, 0.3kg of oleic acid, 5kg of soluble binder, 0.3kg of polyether modified silicone oil and the balance of solvent, and stirring and mixing the materials for 4 hours to obtain slurry, wherein the total weight of the solvent is 100 kg; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming for 35min to obtain the high-solid-content manganese zinc ferrite slurry.
Example 5
The embodiment discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
Taking 100kg of a mixture of a composite dispersing agent, 1.5kg of manganese zinc ferrite powder and 75kg of a solvent, wherein the composite dispersing agent is obtained by mixing calcium gluconate, triethanolamine and sorbitol according to a mass ratio of 1:1:1, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), adding 75kg of the mixture obtained in the step (1) into a ball mill to perform ball milling and mixing to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:550, the ball milling rotating speed is 180r/min, the ball milling time is 150min, the ball-material ratio is 5.5:1, and the granularity D50 of the grinding product A is 1.3 mu m.
Step (3), adding 25kg of the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B; ball milling rotation speed is 1100r/min, ball material ratio is 5.5:1, ball milling time is 110min, and particle size D50 of ground product B is 180nm.
Step (4) taking 4.73kg of paraffin wax, 1.18kg of microcrystalline wax, 1.5kg of stearic acid and 0.97kg of dibutyl phthalate, uniformly mixing at 75 ℃ to obtain soluble composite wax, adding 0.86kg of coupling agent KH560, uniformly stirring, cooling to room temperature, and crushing to obtain the soluble binder.
Step (5) taking 48kg of grinding product A, 26kg of grinding product B, 0.4kg of oleic acid, 9kg of soluble binder, 0.7kg of polyether modified silicone oil and the balance of solvent, and stirring and mixing the materials for 7h to obtain slurry, wherein the total weight of the solvent is 100 kg; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming for 50min to obtain the high-solid-content manganese zinc ferrite slurry.
Comparative example 1
The comparative example discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
Taking 100kg of a mixture of triethanolamine, manganese zinc ferrite powder and solvent, wherein the mixture comprises 0.9kg of triethanolamine, 68kg of manganese zinc ferrite powder and the balance of solvent, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), adding 65kg of the mixture obtained in the step (1) into a ball mill to perform ball milling and mixing to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:450, the ball milling rotating speed is 100r/min, the ball milling time is 80min, the ball-material ratio is 4.5:1, and the granularity D50 of the grinding product A is 1.6 mu m.
Step (3), adding 35kg of the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B; ball milling speed is 900r/min, ball material ratio is 4.5:1, ball milling time is 90min, and particle size D50 of ground product B is 220nm.
Step (4) taking 4.73kg of paraffin wax, 1.18kg of microcrystalline wax, 1.5kg of stearic acid and 0.97kg of dibutyl phthalate, uniformly mixing at 65 ℃ to obtain soluble composite wax, adding 0.46kg of coupling agent KH560, uniformly stirring, cooling to room temperature, and crushing to obtain the soluble binder.
Step (5) taking 44kg of grinding product A, 22kg of grinding product B, 0.3kg of oleic acid, 5kg of soluble binder, 0.3kg of polyether modified silicone oil and the balance of solvent, and stirring and mixing the materials for 4 hours to obtain slurry, wherein the total weight of the solvent is 100 kg; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming for 35min to obtain the high-solid-content manganese zinc ferrite slurry.
Comparative example 2
The comparative example discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
taking 100kg of a mixture of calcium gluconate, manganese zinc ferrite powder and a solvent, wherein the mixture comprises 0.9kg of calcium gluconate, 68kg of manganese zinc ferrite powder and the balance of the solvent, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), adding 65kg of the mixture obtained in the step (1) into a ball mill to perform ball milling and mixing to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:450, the ball milling rotating speed is 100r/min, the ball milling time is 80min, the ball-material ratio is 4.5:1, and the granularity D50 of the grinding product A is 1.6 mu m.
Step (3), adding 35kg of the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B; ball milling speed is 900r/min, ball material ratio is 4.5:1, ball milling time is 90min, and particle size D50 of ground product B is 220nm.
Step (4) taking 4.73kg of paraffin wax, 1.18kg of microcrystalline wax, 1.5kg of stearic acid and 0.97kg of dibutyl phthalate, uniformly mixing at 65 ℃ to obtain soluble composite wax, adding 0.46kg of coupling agent KH560, uniformly stirring, cooling to room temperature, and crushing to obtain the soluble binder.
Step (5) taking 44kg of grinding product A, 22kg of grinding product B, 0.3kg of oleic acid, 5kg of soluble binder, 0.3kg of polyether modified silicone oil and the balance of solvent, and stirring and mixing the materials for 4 hours to obtain slurry, wherein the total weight of the solvent is 100 kg; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming for 35min to obtain the high-solid-content manganese zinc ferrite slurry.
Comparative example 3
The comparative example discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
Taking 100kg of a mixture of sorbitol, manganese zinc ferrite powder and a solvent, wherein the mixture comprises 0.9kg of sorbitol, 68kg of manganese zinc ferrite powder and the balance of the solvent, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), adding 65kg of the mixture obtained in the step (1) into a ball mill to perform ball milling and mixing to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:450, the ball milling rotating speed is 100r/min, the ball milling time is 80min, the ball-material ratio is 4.5:1, and the granularity D50 of the grinding product A is 1.6 mu m.
Step (3), adding 35kg of the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B; ball milling speed is 900r/min, ball material ratio is 4.5:1, ball milling time is 90min, and particle size D50 of ground product B is 220nm.
Step (4) taking 4.73kg of paraffin wax, 1.18kg of microcrystalline wax, 1.5kg of stearic acid and 0.97kg of dibutyl phthalate, uniformly mixing at 65 ℃ to obtain soluble composite wax, adding 0.46kg of coupling agent KH560, uniformly stirring, cooling to room temperature, and crushing to obtain the soluble binder.
Step (5) taking 44kg of grinding product A, 22kg of grinding product B, 0.3kg of oleic acid, 5kg of soluble binder, 0.3kg of polyether modified silicone oil and the balance of solvent, and stirring and mixing the materials for 4 hours to obtain slurry, wherein the total weight of the solvent is 100 kg; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming for 35min to obtain the high-solid-content manganese zinc ferrite slurry.
Comparative example 4
The comparative example discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
Taking 100kg of a mixture of 0.9kg of a composite dispersing agent, 68kg of manganese zinc ferrite powder and the balance of a solvent, wherein the composite dispersing agent is obtained by mixing calcium gluconate, triethanolamine and sorbitol according to a mass ratio of 1:1:1, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), adding 100kg of the mixture obtained in the step (1) into a ball mill to perform ball milling and mixing to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:450, the ball milling rotating speed is 100r/min, the ball milling time is 80min, the ball-material ratio is 4.5:1, and the granularity D50 of the grinding product A is 1.6 mu m.
Step (3) taking 4.73kg of paraffin wax, 1.18kg of microcrystalline wax, 1.5kg of stearic acid and 0.97kg of dibutyl phthalate, uniformly mixing at 65 ℃ to obtain soluble composite wax, adding 0.46kg of coupling agent KH560, uniformly stirring, cooling to room temperature, and crushing to obtain the soluble binder.
Step (4) taking 66kg of grinding product A, 0.3kg of oleic acid, 5kg of soluble binder, 0.3kg of polyether modified silicone oil and the balance of solvent, and stirring and mixing the materials for 4 hours to obtain slurry; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (5) filtering the slurry obtained in the step (4), and carrying out vacuum defoaming for 35min to obtain the high-solid-content manganese zinc ferrite slurry.
Comparative example 5
The comparative example discloses a production process of high-solid-content manganese zinc ferrite slurry, which comprises the following steps:
Taking 100kg of a mixture of 0.9kg of a composite dispersing agent, 68kg of manganese zinc ferrite powder and the balance of a solvent, wherein the composite dispersing agent is obtained by mixing calcium gluconate, triethanolamine and sorbitol according to a mass ratio of 1:1:1, and the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
Step (2), adding 65kg of the mixture obtained in the step (1) into a ball mill to perform ball milling and mixing to obtain a grinding product A; wherein, the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used by the ball mill is 1:450, the ball milling rotating speed is 100r/min, the ball milling time is 80min, the ball-material ratio is 4.5:1, and the granularity D50 of the grinding product A is 1.6 mu m.
Step (3), adding 35kg of the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B; ball milling speed is 900r/min, ball material ratio is 4.5:1, ball milling time is 90min, and particle size D50 of ground product B is 220nm.
Step (4) taking 44kg of grinding product A, 22kg of grinding product B, 0.3kg of oleic acid, 0.58kg of dibutyl phthalate, 0.89kg of stearic acid, 3.53kg of polyvinyl alcohol, 0.3kg of polyether modified silicone oil and the balance of solvent, and stirring and mixing the materials for 4 hours to obtain slurry; wherein the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1.
And (5) filtering the slurry obtained in the step (4), and carrying out vacuum defoaming for 35min to obtain the high-solid-content manganese zinc ferrite slurry.
The Mn-Zn ferrite powder in all the above examples and comparative examples is from Shanghai Huangpu district magnetic-health electronic manager; calcium gluconate, 99% content, from the company of Hunan Tai ren pharmaceutical Co; triethanolamine, CAS number 102-71-6, product number TEA, from Tianjin and Shengtai chemical Co., ltd; sorbitol, CAS number 50-70-4 from Tianjin and Shengtai chemical Co., ltd; xylene content 99 (%) from Tianjin neutralization shengtai chemical company, ltd; paraffin wax, cat# 68, 40 ℃ kinematic viscosity 71.15 from Tianjin and shengtai chemical company, ltd; stearic acid, CAS number 57-11-4, cargo number stearic acid 1801 from Tianjin and Shengtai chemical Co., ltd; microcrystalline wax, cat# 569, cat# 85 microcrystalline wax from the company, inc. Of the color beeswax gum, jean; dibutyl phthalate, CAS84-74-2, cat# 202003210, type DBP plasticizer, available from Jinan Ming Wei chemical Co., ltd; oleic acid from jinan jingruixin chemical industry limited; polyether modified silicone oil with the content of 99 percent and the PH value of 7-8 is obtained from Ministry chemical industry Co., ltd; coupling agent KH560, CAS number 2530-83-8 was from Dongguan mountain-plasticizing Co., ltd, and the active substance content was 99 (%).
Experimental example
Test one, slurry concentration test: the concentration of the high solid content Mn-Zn ferrite slurries prepared in examples 1-5 and comparative examples 1-5 was examined by a baking method.
Testing II, slurry viscosity testing: the viscosity of the high solids manganese zinc ferrite slurries prepared in examples 1-5 and comparative examples 1-5 were tested using a rotary viscometer (model NDJ-1, shanghai Qigao instruments).
The test results are shown in table 1:
TABLE 1
As shown by the test results in the table 1, the slurry solid content of the high-solid-content Mn-Zn ferrite slurry prepared in the embodiment of the invention is above 60%, and the maximum solid content can reach 82%; furthermore, the composite dispersing agent and the soluble binder can promote the dispersibility of solids in slurry, and can improve the solid content and simultaneously keep the slurry of the invention with good fluidity.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The production process of the manganese zinc ferrite slurry with high solid content is characterized by comprising the following steps of:
And (3) proportioning: mixing a mixture of a composite dispersing agent, manganese zinc ferrite powder and a solvent, wherein the composite dispersing agent comprises calcium gluconate, triethanolamine and sorbitol; the mass ratio of each component in the mixture is as follows: 0.5-2% of composite dispersant, 66-79% of manganese zinc ferrite powder and the balance of solvent; the solvent is obtained by mixing ethanol and dimethylbenzene according to a mass ratio of 1:1; the mass ratio of the calcium gluconate to the triethanolamine to the sorbitol in the composite dispersing agent is 1:1:1;
step (2) adding the mixture obtained in the step (1) into a ball mill to perform ball milling and mixing to obtain a ground product A, wherein the granularity D50 of the ground product A is 1.2-1.8 mu m;
Step (3), adding the mixture obtained in the step (1) into a high-energy ball mill to perform ball milling and mixing to obtain a grinding product B, wherein the granularity D50 of the grinding product B is 150-250nm; wherein the ball milling rotating speed is 800-1200r/min, the ball-material ratio is 4-6:1, and the ball milling time is 80-120min;
step (4) taking paraffin, microcrystalline wax, stearic acid and dibutyl phthalate, heating and mixing until uniformity is achieved, obtaining soluble composite wax, adding a coupling agent, stirring uniformly, cooling to room temperature, and crushing to obtain a soluble binder;
Step (5) taking the grinding product A, the grinding product B, a dispersing agent, a soluble binder, a defoaming agent and a solvent, and stirring and mixing to obtain slurry; wherein, the mass ratio of each component in the slurry is as follows: 42-50% of grinding product A, 20-28% of grinding product B, 0.25-0.5% of dispersing agent, 3.5-11% of soluble binder, 0.1-1% of defoaming agent and the balance of solvent;
and (6) filtering the slurry obtained in the step (5), and carrying out vacuum defoaming to obtain the manganese zinc ferrite slurry with high solid content.
2. The process for producing the high-solid-content manganese-zinc-ferrite slurry according to claim 1, wherein in the step (2), the number ratio of the bearing steel balls with the diameter of 6mm to the bearing steel balls with the diameter of 4.8mm used in the ball mill is 1:400-600, the ball milling rotating speed is 60-240r/min, the ball milling time is 60-180min, and the ball-material ratio is 4-6:1.
3. The process for producing a high solid content manganese zinc ferrite slurry according to claim 1, wherein in the step (4), the mass ratio of paraffin wax, microcrystalline wax, stearic acid and dibutyl phthalate is 4.73:1.18:1.5:0.97, and the heating temperature is 60-80 ℃.
4. The process for producing the high-solid-content manganese-zinc-ferrite slurry according to claim 1, wherein in the step (4), a coupling agent KH560 is adopted as a coupling agent, and the mass ratio of the coupling agent to the paraffin is 4.73:0.26-1.06.
5. The process for producing high solids content Mn-Zn ferrite slurry according to claim 1, wherein in the step (5), the slurry mixing time is 3-10 hours.
6. The process for producing a high solids content Mn-Zn ferrite slurry according to claim 1, wherein the vacuum degassing time in the step (6) is 30 to 60 minutes.
7. A high solids manganese zinc ferrite slurry prepared by the process of any one of claims 1-6.
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| CN101844914A (en) * | 2010-05-11 | 2010-09-29 | 武汉吉磁电子科技有限责任公司 | Magnetoplumbate-type permanent magnetic ferrite and manufacturing method thereof |
| CN111995384A (en) * | 2020-07-28 | 2020-11-27 | 浙江工业大学 | Preparation method of high-solid-content high-performance injection-molded nickel-zinc ferrite particles and sintered magnet |
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| CN101844914A (en) * | 2010-05-11 | 2010-09-29 | 武汉吉磁电子科技有限责任公司 | Magnetoplumbate-type permanent magnetic ferrite and manufacturing method thereof |
| CN111995384A (en) * | 2020-07-28 | 2020-11-27 | 浙江工业大学 | Preparation method of high-solid-content high-performance injection-molded nickel-zinc ferrite particles and sintered magnet |
| CN113716950A (en) * | 2021-11-01 | 2021-11-30 | 天通控股股份有限公司 | Low-temperature sintered flexible magnetic sheet and preparation method thereof |
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