CN100395850C - Method for preparing binded NdFeB in-situ after injection moulding forming - Google Patents
Method for preparing binded NdFeB in-situ after injection moulding forming Download PDFInfo
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- CN100395850C CN100395850C CNB2005100372908A CN200510037290A CN100395850C CN 100395850 C CN100395850 C CN 100395850C CN B2005100372908 A CNB2005100372908 A CN B2005100372908A CN 200510037290 A CN200510037290 A CN 200510037290A CN 100395850 C CN100395850 C CN 100395850C
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Abstract
The present invention discloses a method for preparing bond NdFeB magnet in-situ polymerization after injection moulding. In the method, NdFeB magnetic powder which is treated by coating is added in caprolactam monomer solution to make intermediate reaction bodies, the intermediate reaction bodies can be directly injected into a mold cavity by utilizing a twin-screw extruder or a single-screw extruder, and polymer agglomerant can be formed and moulded at the surface of the magnetic powder by in-situ polymerization reaction. Magnetic powder agglomerant mixing and magnet moulding can be completed by one step by the method, the processes of granulation and granules reheating are omitted, the moulding process of the injection for preparing bond NdFeB magnet is simplified, and the investment of granulation devices is saved. The polymer which is used as agglomerant is also generated at the surface of the magnetic powder by the method, one layer of polymer is uniformly coated on the surface of each magnetic powder, so the magnetic powder can be reliably combined with the agglomerant, and fully uniform mixing of magnetic powder and the agglomerant is ensured on technically.
Description
Technical field
The present invention relates to magnet forming processing technology field, specifically be meant the method preparation bonding NdFeB magnet of in-situ after injection moulding.
Background technology
Bonding NdFeB magnet be will be with the NdFeB magnetic of quick quenching technique or the preparation of HDDR method and resin or macromolecular material mixing after, make after with mold pressing, injection moulding, rolling process etc. it being prepared into final size and shape.Bonded permanent magnet because have that cost is low, dimensional accuracy is high, freedom shape is big, mechanical strength is good, light specific gravity, can automated production in enormous quantities continuously, the production efficiency height, advantages such as good product consistency, industry, agricultural, military affairs, science and technology, medical science, life various aspects have been widely used in, the spindle motor of for example a large amount of miniature precision electric motors that use, stepping motor, hard disk drive etc.Wherein, bonding NdFeB magnet accounts for 94% of total output in the application quantity maximum of rotary device (mainly being the electrical micro-machine that computer is used).
Injection moulding bonded permanent magnet body technology is that the permanent magnetism powder with certain particle size mixes with binding agent that (binding agent can account for 30%, volume fraction) carries out granulation after, in injector, to be heated to uniform temperature through the magnetic of granulation is injected to powder in the die cavity by an aperture with screw rod again, magnetic is squeezed into required form in die cavity, and in die cavity, cool off and curing, obtain the bonded permanent magnet of required size and shape.Can be used for injection molding magnetic has the mixed powder etc. of NdFeB, SmCo, ferrite, Alnico and above-mentioned several powder, and wherein the magnetic of injection moulding bonding NdFeB magnet is the highest.According to the used magnetic and the difference of technology, the injection magnet has the branch of isotropism and anisotropy again.
The injection moulding bonded permanent magnet has following several characteristics:
(1) magnet shape degree of freedom height.Can prepare comparatively complicated shape, as motor with thin-walled ring bonded permanent magnet.If use die pressing, then be difficult to preparation.
(2) dimensional accuracy height.Adopt the injection molding of high dimensional accuracy to make high accuracy injection moulding bonded permanent magnet, do not need the back processing as sintered magnet, product can directly be used in precision optical machinery and automobile with on the device.
(3) cost is lower than compression molding method.To compare processing step few with die pressing, the efficient height, but and a plurality of magnets of a shot, therefore, have lower technology cost.
(4) can carry out combination forming.Utilize injection molding technology bonded permanent magnet and metalwork can be combined and carry out one-shot forming, form embedded assembling device, realize the shape variation, complicated of moulding article assembly.This is the great advantage of injection moulding bonded permanent magnet.
As mentioned above, the injection molding technique process of bonded permanent magnet mainly comprises: (1) is carried out the surface to magnetic and is coated processing; (2) magnetic and binding agent are mixed,, obtain dry pellet through mixing and granulation; (3) pellet is delivered to the heating chamber heating with spiral guide bar, be injected into mould molding, promptly get product after the cooling.Concrete technological process is as follows:
Magnaglo+binding agent+additive → mixing, granulation → injection (mo(u)lding) machine → matched moulds → injection injection → cooling → die sinking → oriented moulding → demagnetize → magnetize.
Polyamide (nylon) is a kind of binding agent the most frequently used in the injection molding technique of bonded permanent magnet, and addition generally is 20～30% (percentage by volumes).
There is following deficiency in prior art: after (1) prior art adopts surface treated NdFeB magnetic and polyamide (nylon), lubricant, antioxidant mixed in high-speed mixer by a certain percentage, in twin-screw (single screw rod) extruder, melt extrude, granulation, injection molding production technology in injection molding machine then, complex technical process; (2) prior art all adopts magnetic and the direct hybrid technique of binding agent, and the density of NdFeB magnetic is 7.64g/cm
3, the density of nylon is 1.11g/cm
3,, mixing apparatus is required high because the difference of magnetic and polymer proportion in order to make two kinds of material mixing even, must be carried out high speed, high strength mixing; (3) form of mainly utilizing coupling agent to pass through chemical bond between inorganic magnetic and the organic binder bond combines, and bond strength is low, also can the uniformity of mixing between magnetic and the binding agent be exerted an influence.
Summary of the invention
Purpose of the present invention is exactly in order to solve above-mentioned the deficiencies in the prior art part, proposition utilizes the method preparation bonding NdFeB magnet of in-situ after injection moulding, realize that the magnetic binding agent mixes and the magnet forming process is once finished, simplify the technical process of injection preparation bonding NdFeB magnet and reduce the purpose of using equipment requirements and strengthening magnetic and binding agent bond strength.
The present invention is achieved through the following technical solutions: described in-situ after injection moulding method preparation bonding NdFeB magnet comprises the steps and process conditions:
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 1～5 part coupling agent and 95～99 parts, coats processing the NdFeB magnetic is carried out surface;
Second step was heated to 70～90 ℃ with caprolactam monomer (CL) and is fused into liquid, was evacuated to 1 * 10
-4～1 * 10
-1Pa dewatered 10～30 minutes;
The 3rd step, charging under the condition of nitrogen gas, in mass fraction, 1098,5～10 parts of HMPAs of 0.1～0.3 part of anti-oxidant Irganox (HPT), 0.5～2 part of lubricant are joined in the caprolactam melt of 100 part of second step preparation, make monomer solution; Subsequently 7～15 parts of described monomer solutions are mixed with 85～93 parts of magnetics of handling through first step coating, stir, make mixed system; In 100 parts of described mixed systems, add 0.1～0.5 part toluene diisocyanate (TDI), 0.2～0.8 part initator, be heated to 130～150 ℃ after stirring, be incubated 2～5 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 130～150 ℃ is injected in the mould that is preheating to 160～200 ℃ with twin screw or single screw extruder, be incubated 0.5～4 hour, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon (MC) built-up magnet on NdFeB magnetic surface.
Coupling agent that the first step in the technique scheme is used and used lubricant, initator of the 3rd step are general coupling agent, lubricant and initator in such technology, in order to realize the object of the invention better, coupling agent preferred silane coupling agent KH of the present invention～550, KH～560 or KH～570; The preferred potassium hydroxide of described initator, NaOH or sodium methoxide; The preferred zinc stearate of described lubricant, calcium stearate or barium stearate.
In order to realize the object of the invention better, the described condition of nitrogen gas that charges into preferably charged into 0.2～0.8Pa high pure nitrogen the 3rd step in the technique scheme.
The present invention compared with prior art has following advantage and beneficial effect:
1, the present invention utilizes twin-screw (single screw rod) extruder directly magnetic and polymer monomer mixture to be injected die cavity, by home position polymerization reaction polymeric binder is formed and moulding on the magnetic surface, the magnetic binding agent was mixed with one step of magnet forming process to be finished, save granulation and pellet reheats process, simplify the molding process of injection preparation bonding NdFeB magnet, saved the Granulation Equipments investment;
2, the present invention mixes the NdFeB magnetic with polymer monomer, utilize the home position polymerization reaction technology, polymer as binding agent is generated at the magnetic surface in situ, coated equably the one layer of polymeric on the surface of every magnetic, make magnetic with as the polymer reliable connection of binding agent, guaranteed that from technology magnetic mixes with the full and uniform of binding agent.
Embodiment
Below in conjunction with embodiment, the present invention is done detailed description further, but embodiments of the present invention are not limited thereto.
Embodiment one
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 1 part KH550 and 99 parts, coats processing the NdFeB magnetic is carried out surface;
Second step was heated to 80 ℃ with caprolactam monomer (CL) and is fused into liquid, was evacuated to 1 * 10
-1Pa dewatered 30 minutes;
The 3rd step charging under the 0.2Pa high pure nitrogen condition, in mass fraction, added 0.15 part of 1098,5 parts of HMPA of anti-oxidant Irganox (HPT), 2 parts of calcium stearates in the caprolactam melt of 100 part of second step preparation, make monomer solution; The 93 part NdFeB magnetics of 7 parts of monomer solutions with first step preparation are mixed, stir, make mixed system; In 100 parts of mixed systems, add 0.5 part toluene diisocyanate (TDI), 0.8 part potassium hydroxide, be heated to 150 ℃ after stirring, be incubated 5 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 150 ℃ is injected into rapidly in the mould that is preheating to 200 ℃ with double screw extruder, be incubated 0.5 hour, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon (MC) built-up magnet on NdFeB magnetic surface.After testing, the density of built-up magnet is 5.2g/cm
3, bending strength 30MPa, maximum magnetic energy product 52kJ/m
3
Embodiment two
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 3 parts KH550 and 93 parts, coats processing magnetic is carried out surface;
Second step was heated to 60 ℃ with caprolactam monomer (CL) and is fused into liquid, was evacuated to 1 * 10
-4Dewatered 10 minutes;
In the 3rd step, charging under the 0.6Pa high pure nitrogen condition; In mass fraction, in the caprolactam melt of 100 part of second step preparation, add 0.1 part of 1098,7 parts of HMPA of anti-oxidant Irganox (HPT), 1 part of zinc stearate, make monomer solution; The NdFeB magnetic of 10 parts of monomer solutions with 90 parts of first step preparations mixed, stir, make mixed system; In 100 parts of mixed systems, add 0.3 part toluene diisocyanate (TDI), 0.5 part potassium hydroxide, be heated to 140 ℃ after stirring, be incubated 3 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 140 ℃ is injected into rapidly in the mould that is preheating to 180 ℃ with single screw extrusion machine, be incubated 3 hours, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon (MC) built-up magnet on NdFeB magnetic surface.After testing, the density of built-up magnet is 4.7g/cm
3, bending strength 45MPa, maximum magnetic energy product 40kJ/m
3
Embodiment three
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 5 parts KH550 and 95 parts, coats processing magnetic is carried out surface;
Second step was heated to 70 ℃ with caprolactam monomer (CL) and is fused into liquid, was evacuated to 1 * 10
-3Dewatered 15 minutes;
The 3rd step is under the condition that charges into the 0.4Pa high pure nitrogen; In mass fraction, in the caprolactam melt of 100 part of second step preparation, add 0.3 part of 1098,10 parts of HMPA of anti-oxidant Irganox (HPT), 0.5 part of barium stearate, make monomer solution; The NdFeB magnetic of 15 parts of monomer solutions with 85 parts of first step preparations mixed, stir, make mixed system; In 100 parts of mixed systems, add 0.1 part toluene diisocyanate (TDI), 0.2 part potassium hydroxide, be heated to 130 ℃ after stirring, be incubated 2 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 130 ℃ is injected into rapidly in the mould that is preheating to 160 ℃ with double screw extruder, be incubated 4 hours, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon (MC) built-up magnet on NdFeB magnetic surface.After testing, the density of built-up magnet is 4.2g/cm
3, bending strength 70MPa, maximum magnetic energy product 32kJ/m
3
Embodiment four
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 1 part KH560 and 99 parts, coats processing magnetic is carried out surface;
Second step was heated to 80 ℃ with caprolactam monomer (CL) and is fused into liquid, was evacuated to 1 * 10
-1Pa dewatered 30 minutes;
The 3rd step, under the condition that charges into the 0.8Pa high pure nitrogen, in mass fraction, in the caprolactam melt of 100 part of second step preparation, add 0.25 part of 1098,6 parts of HMPA of anti-oxidant Irganox (HPT), 1 part of calcium stearate, make monomer solution; The NdFeB magnetic of 8 parts of monomer solutions with 92 parts of first step preparations mixed, stir, make mixed system; In 100 parts of mixed systems, add 0.45 part toluene diisocyanate (TDI), 0.65 part sodium methoxide, be heated to 150 ℃ after stirring, be incubated 5 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 150 ℃ is injected into rapidly in the mould that is preheating to 180 ℃ with double screw extruder, be incubated 2 hours, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon (MC) built-up magnet on NdFeB magnetic surface.After testing, the density of built-up magnet is 5.0g/cm
3, bending strength 38MPa, maximum magnetic energy product 48kJ/m
3
Embodiment five
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 3 parts KH560 and 97 parts, coats processing magnetic is carried out surface;
Second step was heated to 80 ℃ with caprolactam monomer (CL) and is fused into liquid, was evacuated to 3 * 10
-3Pa dewatered 15 minutes;
The 3rd step is under the condition that charges into the 0.5Pa high pure nitrogen; In mass fraction, in the caprolactam melt of 100 part of second step preparation, add 0.18 part of 1098,10 parts of HMPA of anti-oxidant Irganox (HPT), 1 part of zinc stearate, make monomer solution; The NdFeB magnetic of 12 parts of monomer solutions with 88 parts of first step preparations mixed, stir, make mixed system; In 100 parts of mixed systems, add 0.35 part toluene diisocyanate (TDI), 0.45 part sodium methoxide, be heated to 140 ℃ after stirring, be incubated 3 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 140 ℃ is injected into rapidly in the mould that is preheating to 175 ℃ with single screw extrusion machine, be incubated 2 hours, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon (MC) built-up magnet on NdFeB magnetic surface.After testing, the density of built-up magnet is 4.4g/cm
3, bending strength 50MPa, maximum magnetic energy product 36kJ/m
3
Embodiment six
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 5 parts KH560 and 95 parts, coats processing magnetic is carried out surface;
Second step was fused into liquid for 75 ℃ with caprolactam monomer (CL) heating, was evacuated to 5 * 10
-4Pa dewatered 13 minutes;
The 3rd step is under the condition that charges into the 0.8Pa high pure nitrogen; In mass fraction, in the caprolactam melt of 100 part of second step preparation, add 0.23 part of 1098,5 parts of HMPA of anti-oxidant Irganox (HPT), 0.5 part of barium stearate, make monomer solution; The NdFeB magnetic of 15 parts of monomer solutions with 85 parts of first step preparations mixed, stir, make mixed system; In 100 parts of mixed systems, add 0.2 part toluene diisocyanate (TDI), 0.2 part sodium methoxide, be heated to 135 ℃ after stirring, be incubated 3 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 135 ℃ is injected into rapidly in the mould that is preheating to 180 ℃ with single screw extrusion machine, be incubated 2.5 hours, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon (MC) built-up magnet on NdFeB magnetic surface.After testing, the density of built-up magnet is 4.2g/cm
3, maximum magnetic energy product 30kJ/m
3
Embodiment 7
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 1 part KH570 and 99 parts, coats processing magnetic is carried out surface;
Second step was heated to 90 ℃ with caprolactam monomer (CL) and is fused into liquid, was evacuated to 7 * 10
-2Pa dewatered 25 minutes;
The 3rd step is under the condition that charges into the 0.6Pa high pure nitrogen; In mass fraction, in the caprolactam melt of 100 part of second step preparation, add 0.27 part of 1098,10 parts of HMPA of anti-oxidant Irganox (HPT), 2 parts of barium stearates, make monomer solution; The 93 part NdFeB magnetics of 7 parts of monomer solutions with first step preparation are mixed, stir, make mixed system; In 100 parts of mixed systems, add 0.5 part toluene diisocyanate (TDI), 0.8 part NaOH, be heated to 145 ℃ after stirring, be incubated 4 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 145 ℃ is injected into rapidly in the mould that is preheating to 190 ℃ with twin-screw (single screw rod) extruder, be incubated 4 hours, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon (MC) built-up magnet on NdFeB magnetic surface.After testing, the density of built-up magnet is 5.1g/cm
3, maximum magnetic energy product 50kJ/m
3
Embodiment 8
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 2.5 parts KH570 and 97.5 parts, coats processing magnetic is carried out surface;
Second step was heated to 70 ℃ with caprolactam monomer (CL) and is fused into liquid, was evacuated to 4 * 10
-3Pa dewatered 15 minutes;
The 3rd step charging into the 0.2Pa high pure nitrogen, in mass fraction, added 0.3 part of 1098,7 parts of HMPA of anti-oxidant Irganox (HPT), 1 part of calcium stearate in the caprolactam melt of 100 part of second step preparation, make monomer solution; The NdFeB magnetic of 10 parts of monomer solutions with 90 parts of first step preparations mixed, stir, make mixed system; In 100 parts of mixed systems, add 0.35 part toluene diisocyanate (TDI), 0.5 part NaOH, be heated to 130 ℃ after stirring, be incubated 5 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 130 ℃ is injected into rapidly in the mould that is preheating to 185 ℃ with twin-screw (single screw rod) extruder, be incubated 2.5 hours, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon (MC) built-up magnet on NdFeB magnetic surface.After testing, the density of built-up magnet is 4.65g/cm
3, maximum magnetic energy product 38kJ/m
3
As mentioned above, can realize the present invention preferably.
Claims (5)
1. the method for preparing binded NdFeB in-situ after injection moulding forming is characterized in that comprising the steps and process conditions:
The first step in mass fraction, mixes the back intensive drying with the NdFeB magnetic of 1～5 part coupling agent and 95～99 parts, coats processing the NdFeB magnetic is carried out surface;
Second step was heated to 70～90 ℃ with caprolactam monomer and is fused into liquid, was evacuated to 1 * 10
-4～1 * 10
-1Pa dewatered 10～30 minutes;
The 3rd step charging under the condition of nitrogen gas, in mass fraction, joined 1098,5～10 parts of HMPAs of 0.1～0.3 part of anti-oxidant Irganox, 0.5～2 part of lubricant in the caprolactam melt of 100 part of second step preparation, made monomer solution; Subsequently 7～15 parts of described monomer solutions are mixed with 85～93 parts of magnetics of handling through first step coating, stir, make mixed system; In 100 parts of described mixed systems, add 0.1～0.5 part toluene diisocyanate, 0.2～0.8 part initator, be heated to 130～150 ℃ after stirring, be incubated 2～5 minutes, make the intermediate reaction body;
The 4th step, the 3rd intermediate reaction body that make of step is heated to after 130～150 ℃ is injected in the mould that is preheating to 160～200 ℃ with twin screw or single screw extruder, be incubated 0.5～4 hour, make caprolactam monomer home position polymerization reaction and moulding take place, make NdFeB magnetic-monomer cast nylon built-up magnet on NdFeB magnetic surface.
2. according to the method for the described preparing binded NdFeB in-situ after injection moulding forming of claim 1, it is characterized in that the coupling agent in the described first step is a silane resin acceptor kh-550, KH-560 or KH-570.
3. according to the method for the described preparing binded NdFeB in-situ after injection moulding forming of claim 1, it is characterized in that the lubricant in described the 3rd step is zinc stearate, calcium stearate or barium stearate.
4. according to the method for the described preparing binded NdFeB in-situ after injection moulding forming of claim 1, it is characterized in that the initator in described the 3rd step is potassium hydroxide, NaOH or sodium methoxide.
5. according to the method for the described preparing binded NdFeB in-situ after injection moulding forming of claim 1, it is characterized in that, charge into condition of nitrogen gas for charging into 0.2～0.8Pa high pure nitrogen described in described the 3rd step.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100593828C (en) * | 2007-04-06 | 2010-03-10 | 浙江工业大学 | Method for preparing NdFeB/PPS injection moulding particle material |
| CN102554240A (en) * | 2010-12-31 | 2012-07-11 | 上海爱普生磁性器件有限公司 | Preparation method for bonded neodymium iron boron permanent magnet granular material |
| CN103258610B (en) * | 2013-05-14 | 2016-02-24 | 厦门建霖工业有限公司 | A kind of magnetic plastic composite material and preparation method thereof |
| CN108231310B (en) * | 2016-12-15 | 2021-05-28 | 北京中科三环高技术股份有限公司 | Preparation method of modified neodymium iron boron magnetic powder, modified neodymium iron boron magnetic powder and neodymium iron boron sintered body |
| CN114456372B (en) * | 2022-01-11 | 2023-06-30 | 滁州杰事杰新材料有限公司 | Cast nylon composite material and preparation method thereof |
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