CN110423468B - High-fluidity high-magnetic-property neodymium iron boron PPS plastic magnetic material and preparation method thereof - Google Patents
High-fluidity high-magnetic-property neodymium iron boron PPS plastic magnetic material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a neodymium iron boron PPS plastic magnetic material with high fluidity and high magnetic performance and a preparation method thereof, belonging to the technical field of magnetic materials. The invention provides a neodymium iron boron PPS plastic magnetic material, which comprises the following preparation raw materials in parts by weight: 50-150 parts of PPS, 850-950 parts of neodymium iron boron magnetic powder, 0.3 part of antioxidant, 0.01-30 parts of EEA, 2 parts of lubricating dispersant and 0-11 parts of silane coupling agent. By adding a proper amount of EEA, the invention can improve the oleophylic property of the surface of the neodymium iron boron magnetic powder, enhance the compatibility of the magnetic powder and PPS and other polymers, and enhance the fluidity of the material, thereby improving the content of the magnetic powder. The results of the examples show that the magnetic powder content of the present invention can be increased to 95 wt.%.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a neodymium-iron-boron PPS plastic magnetic material with high fluidity and high magnetic performance and a preparation method thereof.
Background
Compared with neodymium iron boron PA6 or neodymium iron boron PA12 plastic magnetic materials, the neodymium iron boron PPS (polyphenylene sulfide) plastic magnetic material has better heat resistance, humidity resistance and corrosion resistance, and is widely applied to the fields of computer hard disks, mobile phones, variable-frequency household appliances, executing elements for electric appliances and the like.
However, the flowability of the existing neodymium-iron-boron PPS plastic magnetic material is poor, and along with the increase of the content of magnetic powder, the flowability can be further reduced, so that the smooth processing cannot be realized, therefore, the content of neodymium-iron-boron magnetic powder in the existing neodymium-iron-boron PPS plastic magnetic material is generally difficult to reach 93.5 wt.%, and the further improvement of the magnetic performance is influenced.
Disclosure of Invention
The invention aims to provide a neodymium iron boron PPS plastic magnetic material with high fluidity and high magnetic performance and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a neodymium iron boron PPS plastic magnetic material, which comprises the following preparation raw materials in parts by weight: 50-150 parts of PPS, 850-950 parts of neodymium iron boron magnetic powder, 0.3 part of antioxidant, 0.01-30 parts of EEA, 2 parts of lubricating dispersant and 0-11 parts of silane coupling agent.
Preferably, the antioxidant comprises one or more of Ciba 168, Ciba 1010, Ciba 1076 and Ciba 195.
Preferably, the silane coupling agent comprises one or more of SG-Si900, KH-550, KH-551, KH-560 and KH-570.
Preferably, the remanence of the neodymium iron boron magnetic powder is 7.80-8.20 kG, the magnetic energy product is 12.2-14.0 MGOe, and the intrinsic coercive force is 13.0-17.0 kOe.
The invention provides a preparation method of the neodymium iron boron PPS plastic magnetic material, which comprises the following steps:
mixing neodymium iron boron magnetic powder, a solvent and a silane coupling agent, and carrying out first modification on the neodymium iron boron magnetic powder to obtain a first modified mixture;
mixing the first modified mixture with a lubricating dispersant, an antioxidant and EEA, and carrying out second modification to obtain a second modified mixture;
and mixing the second modified mixture with PPS, and extruding to obtain the neodymium iron boron PPS plastic magnetic material.
Preferably, the time for the first modification and the time for the second modification are independently 10 seconds or more.
Preferably, the equipment adopted by the mixing is a torque rheometer, the mixing time is 30min, the rotating speed is 140rpm, the feeding rotating speed is 20rpm, the current of a main machine of the torque rheometer is 20A, and the four-section temperature of the torque rheometer is set to be 310 ℃, 290 ℃ and 290 ℃.
Preferably, before the mixing, the second modified mixture and the PPS are respectively dried.
Preferably, before mixing the neodymium iron boron magnetic powder, the solvent and the silane coupling agent, drying the neodymium iron boron magnetic powder is further included.
Preferably, the extrusion is followed by pelletizing the extruded material.
The invention provides a neodymium iron boron PPS plastic magnetic material, which comprises the following preparation raw materials in parts by weight: 50-150 parts of PPS, 850-950 parts of neodymium iron boron magnetic powder, 0.3 part of antioxidant, 0.01-30 parts of EEA, 2 parts of lubricating dispersant and 0-11 parts of silane coupling agent. According to the invention, by adding a proper amount of EEA and matching with other raw materials, the oleophylic property of the surface of the neodymium iron boron magnetic powder can be improved, the compatibility of the magnetic powder and PPS and other polymers such as antioxidant and EEA is enhanced, and the fluidity of the material is enhanced, so that the content of the magnetic powder can be increased. The results of the examples show that the magnetic powder content of the present invention can be increased to 95 wt.%.
In addition, the formula of the invention greatly improves the fluidity of the neodymium iron boron PPS plastic magnetic material, so the processing time is more appropriate, and the problem of oxidation of a polymer system is also reduced.
The invention provides a preparation method of the neodymium iron boron PPS plastic magnetic material, which is simple and easy to operate and realize industrial production.
Detailed Description
The invention provides a neodymium iron boron PPS plastic magnetic material, which comprises the following preparation raw materials in parts by weight: 50-150 parts of PPS, 850-950 parts of neodymium iron boron magnetic powder, 0.3 part of antioxidant, 0.01-30 parts of EEA, 2 parts of lubricating dispersant and 0-11 parts of silane coupling agent.
The preparation raw materials of the neodymium iron boron PPS plastic magnetic material comprise 50-150 parts by weight of PPS, and preferably 150 parts by weight. In specific embodiments of the invention, the PPS is specifically 50 parts or 150 parts. The source of the PPS is not particularly required in the present invention, and commercially available products known to those skilled in the art may be used. In the embodiment of the present invention, the PPS is preferably pure PPS resin powder of 0220a9 high toughness and flame retardancy manufactured by japanese treasure corporation.
Based on the weight portion of PPS, the preparation raw material of the neodymium iron boron PPS plastic magnetic material provided by the invention comprises 850-950 portions of neodymium iron boron magnetic powder, and preferably 900-950 portions. In a specific embodiment of the present invention, the neodymium iron boron magnetic powder is specifically 850 parts or 950 parts. In the invention, the remanence of the neodymium iron boron magnetic powder is preferably 7.80-8.20 kG, the magnetic energy product is preferably 12.2-14.0 MGOe, and the intrinsic coercive force is preferably 13.0-17.0 kOe. The invention has no special requirements on the particle size of the neodymium iron boron magnetic powder, and the particle size can be any particle size known in the field. The invention has no special requirement on the source of the neodymium iron boron magnetic powder, and can be obtained by adopting commercial commodities well known to technical personnel in the field, such as XQP14-10, XQP15-10 and XQP16-10 quick-quenching alloy magnetic powder produced by Shenyang new oak magnetic material company Limited; MQP-B magnetic powder and MQP-B magnetic powder produced by McGecko magnetic (Tianjin) Co., Ltd+Magnetic powder, etc.; in a specific embodiment of the present invention, the neodymium-iron-boron magnetic powder is preferably available from MQP-A-10179 magnetic powder manufactured by McGemagnet (Tianjin) Inc.
The preparation raw material of the neodymium iron boron PPS plastic magnetic material comprises 0.3 part of antioxidant by weight based on the weight part of PPS. In the present invention, the antioxidant preferably comprises one or more of Ciba 168, Ciba 1010, Ciba 1076 and Ciba 195, more preferably Ciba 168, under the chemical name tris (2, 4-di-tert-butylphenyl) phosphite. The source of the antioxidant is not particularly required in the present invention, and commercially available products well known to those skilled in the art may be used. In a specific embodiment of the present invention, the antioxidant is preferably available from basf (china) limited.
The raw materials for preparing the neodymium iron boron PPS plastic magnetic material provided by the invention comprise 0.01-30 parts of EEA (ethylene-ethyl acrylate) by weight, preferably 10-30 parts, and more preferably 15-25 parts by weight of PPS. In particular embodiments of the invention, the amount of EEA is 5 parts, 10 parts, 15 parts, 20 parts or 30 parts. The source of the EEA is not particularly limited, and commercially available products known to those skilled in the art may be used, and examples thereof include EEA available under the brand name NUC-6940 or NUC-6970, manufactured by NUC corporation of Japan. The EEA is used for replacing a silane coupling agent, the hydrophilicity of the surface of the magnetic powder is changed into lipophilicity, the compatibility of the magnetic powder and PPS and other high molecules is enhanced, the fluidity of the material is enhanced, and the content of the magnetic powder is favorably improved.
Based on the weight part of PPS, the preparation raw material of the neodymium iron boron PPS plastic magnetic material provided by the invention comprises 2 parts of lubricating dispersant. The source of the lubricating dispersant in the present invention is not particularly limited, and commercially available products known to those skilled in the art may be used. The invention has no special requirement on the specific type of the lubricating dispersant, and can adopt the lubricating dispersant commonly used in the field. In a specific embodiment of the invention, the lubricant dispersant is preferably TAF-A manufactured by Suzhongthailand photochemical assistant, Inc.
The preparation raw material of the neodymium iron boron PPS plastic magnetic material comprises 0-11 parts of silane coupling agent by weight of PPS, and preferably 1-11 parts of silane coupling agent by weight of PPS. In the embodiment of the present invention, the amount of the silane coupling agent is specifically 0 part or 10.28 parts by weight when the volume is reduced to parts by weight. In the present invention, the silane coupling agent preferably includes one or more of SG-Si900, KH-550, KH-551, KH-560 and KH-570. The present invention does not require any particular source of the silane coupling agent, and commercially available products well known in the art may be used. The silane coupling agent can increase the binding force between the neodymium iron boron magnetic powder and PPS.
The invention provides a preparation method of the neodymium iron boron PPS plastic magnetic material, which comprises the following steps:
mixing neodymium iron boron magnetic powder, a solvent and a silane coupling agent, and carrying out first modification on the neodymium iron boron magnetic powder to obtain a first modified mixture;
mixing the first modified mixture with a lubricating dispersant, an antioxidant and EEA, and carrying out second modification to obtain a second modified mixture;
and mixing the second modified mixture with PPS, and extruding to obtain the neodymium iron boron PPS plastic magnetic material.
The neodymium iron boron magnetic powder, the solvent and the silane coupling agent are mixed, and the neodymium iron boron magnetic powder is subjected to first modification to obtain a first modified mixture. In the invention, the solvent is preferably absolute ethyl alcohol, and the liquid-solid ratio of the absolute ethyl alcohol to the neodymium-iron-boron magnetic powder is preferably 25mL: 850-950 g. The invention has no special requirements on the equipment adopted by the mixing. In the embodiment of the invention, the mixing equipment is preferably a XJD-300B type miniature high-speed pulverizer produced by Galaxy instruments and factories in Zingiber Officinale. In the present invention, the mixing is preferably performed under stirring conditions; the rate of mixing is not particularly critical to the present invention and may be achieved using agitation rates well known in the art. In the present invention, the time for the first modification is preferably 10 seconds or more, more preferably 10 seconds to 10min, and still more preferably 1 to 3 min. The first modification time of the invention is calculated from the mixing of neodymium iron boron magnetic powder, solvent and silane coupling agent. In the first modification process, neodymium iron boron magnetic powder is coated by a silane coupling agent.
Before mixing the neodymium-iron-boron magnetic powder, the solvent and the silane coupling agent, the invention preferably also comprises drying the neodymium-iron-boron magnetic powder. In the invention, the drying temperature is preferably 120 ℃, the drying time is preferably 30min, and the drying is preferably carried out by adopting a PH-050A constant temperature drying oven.
After the first modified mixture is obtained, the first modified mixture is mixed with a lubricating dispersant, an antioxidant and EEA for second modification to obtain a second modified mixture.
In the present invention, the mixing is preferably performed under stirring conditions; the rate of mixing is not particularly critical to the present invention and may be at any rate known in the art. The invention has no special requirements on the equipment used for mixing, and the mixing equipment well known in the field can be used. In a specific embodiment of the invention, the mixing equipment is preferably a XJD-300B type miniature high-speed pulverizer produced by Galaxy instruments of Jiangyan City. In the present invention, the time for the second modification is preferably 10 seconds or more, more preferably 10 seconds to 10min, and still more preferably 1 to 3 min. The time for the second modification of the invention is calculated from the mixing of the first modified mixture with the lubricant dispersant, the antioxidant and the EEA. In the second modification process, the surface property of the first modified mixture is further improved, and the subsequent improvement of the compatibility with PPS is facilitated.
After the second modified mixture is obtained, the second modified mixture and PPS are mixed and refined, and the neodymium iron boron PPS plastic magnetic material is obtained after extrusion.
Before mixing, the invention preferably also comprises drying the second modified mixture and the PPS respectively. In the invention, the drying temperature of the second modified mixture is preferably 80 ℃, and the time is preferably 1 h. The second modified mixture is dried by preferably adopting a PH-050A type constant-temperature drying oven. In the invention, the drying of the PPS comprises high-temperature drying and low-temperature drying which are sequentially carried out; the high-temperature drying temperature is preferably 120 ℃, and the time is preferably 3 h; the temperature of the low-temperature drying is preferably 60 ℃, and the time is preferably 12 h. The PPS is dried by preferably adopting a PH-050A type constant temperature drying box. The invention adopts high temperature drying and low temperature drying, which can completely remove the water in PPS.
When the second modified mixture and PPS are mixed, the equipment adopted for mixing is preferably a torque rheometer; the mixing time is preferably 30 min; the mixing speed is preferably 140rpm, the feeding speed is preferably 20rpm, the current of a main machine of the torque rheometer is preferably 20A, and the four-stage temperature setting of the torque rheometer is preferably 310 ℃, 290 ℃ and 290 ℃. The present invention does not require special embodiments of the extrusion, and the present invention preferably utilizes an extrusion die of a torque rheometer for extrusion.
After extrusion, the invention preferably also comprises the step of cutting the extruded material into particles to obtain the neodymium iron boron PPS plastic magnetic material. In the invention, the particle size of the granulated neodymium iron boron PPS plastic magnetic material is preferably 2-6 nm, and more preferably 4-5 nm.
The neodymium iron boron PPS plastic magnetic material with high fluidity and high magnetic performance and the preparation method thereof provided by the invention are described in detail below with reference to the examples, but the invention is not to be construed as being limited by the scope of the invention.
Examples 1 to 7
(1) Magnetic powder and PPS pretreatment
Putting NdFeB magnetic powder with the mark of MQP-A-10179 into a PH-050A type constant temperature drying oven to dry for 30min at 120 ℃;
placing PPS resin with the brand number of 0220A9 into a PH-050A type constant temperature drying oven, drying for 3h at 120 ℃, and drying for 12h at 60 ℃;
(2) mixing process
Setting the NdFeB magnetic powder filling amount according to the formula of Table 1, wherein the mass is M1, adding 25mL of absolute ethyl alcohol, adding a coupling agent SG-Si900 with the mass of M3, and mixing for 1.5min at a high speed by using a XJD-300B high-speed mixer to obtain a first modified mixture; thoroughly cleaning the tank after discharging; then, 2g of TAF lubricating dispersant, 0.3g of Bassfeba 168 and EEA (M2) were added and mixed at high speed for 1.5min to obtain a second modified mixture.
(3) Material drying
And (3) putting the second modified mixture into a PH-050A type constant-temperature drying box, and drying for 1 hour at 80 ℃.
(4) Extruding and granulating
Adding the mixed materials into a torque rheometer, adding PPS resin with the mass of M4, and starting the torque rheometer for scouring; mixing time of the torque rheometer is 30min, mixing speed is as follows: 140rpm, feed rate: 20rpm, host current: 20A, four-stage temperature setting: 310. and at the temperature of 310, 290 and 290 ℃, manually cutting the extruded magnetic strip into particles of about 5mm by using a blade at an extrusion die of a torque rheometer to obtain the neodymium iron boron PPS plastic magnetic material.
Comparative example 1
The difference from examples 1-5 is that EEA is not used, and the specific raw material dosage is shown in Table 1.
Performance testing
The MFR fluidity value of the NdFeB PPS plastic-magnetic material is measured by using a F-F01 type melt index meter under the test condition of 270 ℃ and the load of 10 kg. The NdFeB PPS plastic magnetic material is pressed into a cylindrical magnet with the diameter of 24.87mm multiplied by the thickness of 9.70mm by using a LS0-350 type vertical magnetic field orientation press, the magnetic field orientation current is 80A, the pressure is set to be 80 tons, and the pressure is kept for 2 min. Testing the magnetic properties of the NdFeB PPS cylindrical magnet at room temperature of 25 ℃ by using an MA-8101 type magnetic property comprehensive tester, wherein the magnetic properties comprise residual magnetism Br (mT), coercive force jHc (kA/m) and maximum magnetic energy product (BH) max (kJ/m)3) The test results are shown in Table 1.
TABLE 1 raw material formulation and product properties of the examples and comparative examples
As can be seen from the data of examples 1 to 7 and comparative example 1 in Table 1, the flowability of the product can be improved by adding EEA, the MFR of the comparative example 1 is only 7.4g/10min, and the MFR (melt mass flow rate) of the rubidium-iron-boron magnetic powder obtained by adding EEA is as high as 16.7 to 64.1g/10min, which indicates that the rubidium-iron-boron magnetic powder has better flowability and is more favorable for processing; in addition, the balance torque of the comparative example 1 is as high as 90.2 N.m, while the balance torque of the embodiment of the invention is 36.7-78.4 N.m, which shows that the processing difficulty of the invention is greatly reduced.
In addition, from the results of examples 3 and 6, it is clear that the addition of EEA according to the invention contributes to an increase in the magnetic powder content, which can be as high as 95 wt.%. From the results of examples 6 and 7, it is also understood that the addition of EEA can suitably reduce the amount of the silane coupling agent to be added without greatly affecting the magnetic properties and flowability.
According to the embodiment, the neodymium iron boron PPS plastic magnetic material provided by the invention can improve the oleophylic property of the surface of neodymium iron boron magnetic powder, enhance the compatibility of the magnetic powder and PPS and other high molecules, and enhance the fluidity of the material by adding a proper amount of EEA, so that the content of the magnetic powder can be increased, and the content of the magnetic powder can be as high as 95 wt.%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The neodymium iron boron PPS plastic magnetic material is characterized by comprising the following preparation raw materials in parts by weight: 50-150 parts of PPS, 850-950 parts of neodymium iron boron magnetic powder, 0.3 part of antioxidant, 0.01-30 parts of ethylene-ethyl acrylate, 2 parts of lubricating dispersant and 0-11 parts of silane coupling agent.
2. The ndfeb PPS plastic-magnetic material according to claim 1, wherein the antioxidant comprises one or more of a bar 168, a bar 1010, a bar 1076 and a bar 195.
3. The ndfeb PPS plastic-magnetic material according to claim 1, wherein the silane coupling agent comprises one or more of SG-Si900, KH-550, KH-551, KH-560 and KH-570.
4. The ndfeb PPS plastic-magnetic material as claimed in claim 1, wherein the remanence of the ndfeb magnetic powder is 7.80-8.20 kG, the magnetic energy product is 12.2-14.0 MGOe, and the intrinsic coercive force is 13.0-17.0 kOe.
5. The preparation method of the neodymium iron boron PPS plastic magnetic material as claimed in any one of claims 1 to 4, comprising the following steps:
mixing neodymium iron boron magnetic powder, a solvent and a silane coupling agent, and carrying out first modification on the neodymium iron boron magnetic powder to obtain a first modified mixture;
mixing the first modified mixture with a lubricating dispersant, an antioxidant and ethylene-ethyl acrylate, and carrying out second modification to obtain a second modified mixture;
and mixing the second modified mixture with PPS, and extruding to obtain the neodymium iron boron PPS plastic magnetic material.
6. The method according to claim 5, wherein the time for the first modification and the time for the second modification are independently 10 seconds or more.
7. The preparation method according to claim 5, wherein the mixing equipment is a torque rheometer, the mixing time is 30min, the rotating speed is 140rpm, the feeding rotating speed is 20rpm, the current of a main machine of the torque rheometer is 20A, and the four-stage temperature of the torque rheometer is set to be 310 ℃, 290 ℃ and 290 ℃.
8. The preparation method of claim 5, further comprising drying the second modified mixture and PPS separately before mixing.
9. The method according to claim 5, further comprising drying the ndfeb magnetic powder before mixing the ndfeb magnetic powder, the solvent and the silane coupling agent.
10. The method of claim 5, wherein the extruding further comprises cutting the extruded material into pellets.
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| CN114806157B (en) * | 2022-04-29 | 2023-12-01 | 宁波京磁科技发展有限公司 | Neodymium-iron-boron magnetic composite material and preparation method thereof |
| CN116178956B (en) * | 2023-02-17 | 2023-10-13 | 北矿磁材科技有限公司 | Modified PPS, preparation method and application thereof, ferrite/modified PPS plastic magnetic material |
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