CN100593828C - Method for preparing NdFeB/PPS injection moulding particle material - Google Patents

Method for preparing NdFeB/PPS injection moulding particle material Download PDF

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Publication number
CN100593828C
CN100593828C CN200710067880A CN200710067880A CN100593828C CN 100593828 C CN100593828 C CN 100593828C CN 200710067880 A CN200710067880 A CN 200710067880A CN 200710067880 A CN200710067880 A CN 200710067880A CN 100593828 C CN100593828 C CN 100593828C
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ndfeb
magnetic
pps
injection moulding
mass parts
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CN101281811A (en
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姜力强
乔梁
郑精武
盛嘉伟
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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Abstract

The present invention relates to a method for producing a high-performance NdFeB/PPS injection molded grain material, which comprises the following steps: dissolving 0.5-2 parts (by weight) of coupling agent in alcohol, adding 100 parts (by weight) of NdFeB magnetic powder, mixing, drying at 40-60 DEG C, grinding and crushing, and then sieving, to obtain coupled NdFeB magnetic powder; dissolving 0.5-2 parts (by weight) of polyvinyl alcohol in deionized water to form clear solution, adding the coupled NdFeB magnetic powder and PPS resin at a certain proportion into the solution, mixing, and drying thoroughly, grinding and crushing, and sieving the dry compound into grains; compounding the grain material, and then cutting, to obtain the NdFeB/PPS injection molded grain material. The NdFeB/PPS injection molded grain material produced doesn't have the phenomenon of separation between NdFeB magnetic powder and PPS resin in the compounding process, can prevent oxidation of the magnetic powder at high temperature, and therefore greatly improves the performance of the injection molded grain material; the producing method is simple and easy to operate.

Description

A kind of preparation method of NdFeB/PPS injection moulding particle material
(1) technical field
The present invention relates to the preparation method of high performance Nd FeB/PPS injection moulding particle material, belong to the composite magnetic manufacture field.
(2) background technology
Injection moulding neodymium iron boron (NdFeB) built-up magnet be with the NdFeB magnetic of quick quenching technique or HDDR method preparation and macromolecular material carry out mixing, prepare particulate material through extruding pelletizing, pass through the built-up magnet that the injection moulding processing and preparing becomes various whole size and dimensions then.Because injection moulding neodymium iron boron (NdFeB) built-up magnet has magnetic property excellence, dimensional accuracy height, suitable production in enormous quantities, easy-formation complicated shape magnet, advantages such as good mechanical property, the development trend that meets electronic information machine product " light, thin, short, little ", be widely used in many aspects such as household electrical appliance, automobile, communication equipment, detecting instrument, computer, office equipment, thereby be subjected to extensive attention.Macromolecular material is used nylon (PA) series usually, but injection moulding NdFeB/PA built-up magnet is restricted at precision instrument and high temperature field because of maximum magnetic energy product is low and thermal stability is relatively poor.And that polyphenylene sulfide (PPS) has is high temperature resistant, compatibility good, low water absorption, high advantages such as dimensional stability, can satisfy the market demand of high temperature resistant environment (as automotive field) with its injection moulding NdFeB/PPS built-up magnet for preparing.
The technical process of traditional preparation process injection moulding NdFeB/PPS built-up magnet is as follows:
NdFeB magnetic+Powdered PPS resin → mixing processing → extrude pelletizing obtains particulate material → injection moulding+magnetic field orientating → demoulding → magnetize → NdFeB/PPS built-up magnet product.
Wherein the particulate material of processability excellence is to make the key of injection moulding NdFeB/PPS built-up magnet.And full and uniform mix of two kinds of materials of NdFeB and PPS before mixing is the key that obtains the excellent properties particulate material.
There is following deficiency in present existing technology: 1. high magnetic filling rate is one of the prerequisite that improves the magnetic property of built-up magnet, and NdFeB magnetic volume ratio arrives 70% when therefore requiring batch mixing, but the density (7.6g/cm of NdFeB 3) be far longer than PPS (1.3g/cm again 3) density of resin, therefore, according to prior art, when adopting high magnetic filling rate, two kinds of powders carry out often occurring in the mixing process phenomenon that NdFeB separates with PPS in charging respectively, this causes the mixing mix ingredients that goes out inhomogeneous, and directly the particulate material outward appearance (coarse as outward appearance) and the performance (all descending as rheological characteristic and magnetic property) of pelletizing are extruded in influence, thereby influence the performance of final products.2. because mixing process is to carry out under high temperature (greater than 300 ℃), and the NdFeB magnetic is mixing with regard to directly carrying out without any surface treatment, this must cause the severe oxidation of magnetic, thereby also influences the performance of particulate material and final products.
(3) summary of the invention
The objective of the invention is to solve that NdFeB magnetic and pulverous PPS resin mix inhomogeneous and the deficiency easy oxidation of magnetic in the prior art in mixing process, a kind of method of making high performance Nd FeB/PPS injection moulding particle material is provided, realizes mixing uniform purpose.
The technical solution used in the present invention is as follows:
A kind of preparation method of NdFeB/PPS injection moulding particle material, carry out as follows:
(1) coupling processing: 0.5~2 mass parts coupling agent is dissolved with alcohol, add 100 mass parts NdFeB magnetics then, the consumption of alcohol is enough to soak into the NdFeB magnetic, mixing, then 40~60 ℃ of following intensive dryings, grind broken, screening, obtain coupling NdFeB magnetic, described coupling agent is a titante coupling agent;
(2) pre-granulation: get coupling NdFeB magnetic 100 mass parts that step (1) makes, the polyvinyl alcohol of 0.5~2 mass parts is dissolved in the deionized water, form clear solution, in described clear solution, add pulverous PPS resin of the coupling NdFeB magnetic of getting and 8~12 mass parts, mix, 70~90 ℃ of following intensive dryings, cooling is taken out grinding and is broken into particulate material then;
(3) mixing, the pelletizing acquisition NdFeB/PPS injection moulding particle material of the particulate material that step (2) is obtained.
The NdFeB magnetic is passed through coupling processing in advance, can make the magnetic powder particle surface coat one deck coupling agent polymeric membrane, so not only prevent the oxidation of NdFeB magnetic when high-temperature mixing, and, promote hydrophilic NdFeB to combine with oil loving PPS is better by the high molecular coupled action of performance coupling agent.
Pre-prilling is handled and can be made NdFeB magnetic and pulverous PPS resin just mix before mixing full and uniformly, thereby can avoid two components to cause the phenomenon of separation because of the density difference when mixing.Simultaneously, the polyvinyl alcohol that adds in pre-prilling covers the surface of NdFeB magnetic, also can further prevent the oxidation of NdFeB.
Further, described coupling agent is NXT102.
Further again, the alcohol described in the step (1) taking cost into account is preferably absolute ethyl alcohol.
After the intensive drying cooling, take out the grinding fragmentation and obtain particulate material in the step (2), particle diameter helps follow-up mixing, pelletizing technology preferably to 5mm and following.
In the method, generally can prepare by quick quenching technique or HDDR method as the described NdFeB magnetic of raw material, this method is applicable to other isotropism and anisotropy NdFeB magnetic simultaneously.
Concrete, the preparation method of described NdFeB/PPS injection moulding particle material carries out according to following steps:
The NdFeB magnetic that quick quenching technique is obtained carries out coupling processing: with the coupling agent anhydrous alcohol solution of 0.5~2 mass parts, the fast quenching NdFeB magnetic that adds 100 mass parts, the amount of absolute ethyl alcohol is just soaked the NdFeB magnetic, under ventilation condition, constantly stir, fully mix magnetic and coupling agent, then 40~60 ℃ of following intensive dryings, being cooled to room temperature takes out, grind broken, screening, obtain coupling fast quenching NdFeB magnetic, described coupling agent is NXT102;
Pre-granulation is handled: the polyvinyl alcohol of 0.5~2 mass parts is dissolved in forms colourless transparent solution in the deionized water; the Powdered PPS resin that adds 100 mass parts coupling fast quenching NdFeB magnetics and 8~12 mass parts again; constantly stir simultaneously; magnetic, PPS resin are mixed with polyvinyl alcohol evenly; 70~90 ℃ of following intensive dryings; be cooled to room temperature taking-up grinding and be broken into the particulate material that particle diameter is not more than 5mm, the particulate material that obtains is mixing, pelletizing obtains the NdFeB/PPS injection moulding particle material.
With respect to existing method; the NdFeB magnetic that quick quenching technique or HDDR method are obtained has carried out coupling processing before directly mixing and pre-granulation is handled; carry out again afterwards mixing, extrude pelletizing, specifically can with pre-granulation material through mill extruder or double screw extruder carry out mixing, extrude pelletizing and obtain the NdFeB/PPS injection moulding particle material.
Afterwards, the NdFeB/PPS injection moulding particle material of available the present invention preparation carries out other processing, as injection moulding, magnetic field orientating, the demoulding, magnetize, obtains NdFeB/PPS built-up magnet product.
The present invention compared with prior art, its beneficial effect is embodied in:
The NdFeB/PPS injection moulding particle material of the present invention's preparation, when mixing, be not prone to the phenomenon that the NdFeB magnetic separates when mixing with the PPS resin, and prevented the oxidation of magnetic under the high temperature, this has improved the performance of NdFeB/PPS injection moulding particle material greatly, for the injection moulding NdFeB/PPS built-up magnet of processability excellence lays the foundation, the preparation method is simple, and is easy to operate.
(4) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
Get 100g titanate coupling agent NXT102 anhydrous alcohol solution, add 20Kg fast quenching NdFeB magnetic then, the amount of absolute ethyl alcohol is advisable just to soak fast quenching NdFeB magnetic, under ventilation condition, constantly stir, make magnetic fully mix with coupling agent, 50 ℃ of following intensive dryings, be cooled to room temperature and take out broken, the screening of grinding then, obtain coupling fast quenching NdFeB magnetic.
The 100.5g polyvinyl alcohol is dissolved in the deionized water, form colourless transparent solution, add then and go up step coupling fast quenching NdFeB magnetic and the pulverous PPS resin of 2412g, under ventilation condition, constantly stir, make magnetic, PPS resin fully mix with polyvinyl alcohol, 80 ℃ of following intensive dryings, be cooled to room temperature and take out broken, the screening of grinding then, obtain the following pre-granulation material of size 5mm.
The 3rd step, will be above-mentioned pre-granulation material through the mill extruder carry out mixing, extrude pelletizing acquisition NdFeB/PPS injection moulding particle material.Randomly draw three batch of materials (every crowd of 2Kg is labeled as A, B, C respectively) then and carry out injection moulding, being prepared into diameter is 12cm, highly is the cylindrical sample of 10cm, measures the magnetic property of this cylindrical sample then with the permanent magnetism tester, the results are shown in Table 1.
The magnetic property of table 1 NdFeB/PPS composite material
Br,Gs Hcb,Oe Hcj,Oe (BH)max,MGOe The sampling batch
4950 4080 8850 5.10 A
4960 4090 8850 5.11 B
4960 4110 8940 5.13 C
Embodiment 2: Comparative Examples
Get 100g titanate coupling agent NXT102 anhydrous alcohol solution, add 20Kg fast quenching NdFeB magnetic then, the amount of absolute ethyl alcohol is advisable just to soak fast quenching NdFeB magnetic, under ventilation condition, constantly stir, make magnetic fully mix with coupling agent, 50 ℃ of following intensive dryings, be cooled to room temperature and take out broken, the screening of grinding then, obtain coupling fast quenching NdFeB magnetic.
To go up step coupling fast quenching NdFeB magnetic and the pulverous PPS resin of 2412g, through the mill extruder carry out mixing, extrude pelletizing and obtain the NdFeB/PPS injection moulding particle material.Operation sampling according to the 3rd step of embodiment 1 obtains the cylinder standard component and tests its magnetic property through injection moulding.The results are shown in Table 2.
Embodiment 3: Comparative Examples
To mix without the fast quenching NdFeB magnetic 20Kg and the pulverous PPS resin of 2400g of coupling processing, through the mill extruder carry out mixing, extrude pelletizing and obtain the NdFeB/PPS injection moulding particle material.Operation sampling according to the 3rd step of embodiment 1 obtains the cylinder standard component and tests its magnetic property through injection moulding.The results are shown in Table 2.
Embodiment 2~3 adopts fast quenching NdFeB isotropism magnetic.
The magnetic property of table 2 NdFeB/PPS composite material
Br,Gs Hcb,Oe Hcj,Oe (BH)max,MGOe
Embodiment 2 4860 3970 8360 4.87
Embodiment 3 4530 3550 8050 4.12
From table 1~2 as can be seen, among the embodiment 1 each sample magnetic property change little, the A that obtains at random, B, C three batch of material performance unanimities, this shows that also the uniformity of this particulate material and consistency are fine.From the comparing result of embodiment 1 and 2, through pre-prilling, the magnetic property of injection moulding NdFeB magnet obviously improves, and it is relevant that the coating of this and polyvinyl alcohol has reduced the NdFeB surface oxidation degree.From the comparing result of embodiment 1 and 3, it is a lot of to descend through the magnetic property of the magnet of coupling process and pre-prilling, this with mixing process in magnetic and PPS resin isolation cause that the composition deviation is relevant.
Embodiment 4~11
Get 0.5~2 mass parts titanate coupling agent NXT102 anhydrous alcohol solution, add 20Kg fast quenching NdFeB magnetic then, the amount of absolute ethyl alcohol is advisable just to soak fast quenching NdFeB magnetic, under ventilation condition, constantly stir, make magnetic fully mix with coupling agent, 50 ℃ of following intensive dryings, be cooled to room temperature and take out broken, the screening of grinding then, obtain coupling fast quenching NdFeB magnetic.
The polyvinyl alcohol of 0.5~2 mass parts is dissolved in the deionized water, form colourless transparent solution, add then and go up step coupling fast quenching NdFeB magnetic and the pulverous PPS resin of 8~12 mass parts, under ventilation condition, constantly stir, make magnetic, PPS resin fully mix with polyvinyl alcohol, 80 ℃ of following intensive dryings, be cooled to room temperature and take out broken, the screening of grinding then, obtain the following pre-granulation material of size 5mm.
The amount of NXT102, NdFeB magnetic, polyvinyl alcohol and the PPS resin that adds at each embodiment is as shown in table 3.
The 3rd step, will be above-mentioned pre-granulation material through the mill extruder carry out mixing, extrude pelletizing acquisition NdFeB/PPS injection moulding particle material.Operation sampling according to the 3rd step of embodiment 1 obtains the cylinder standard component and tests its magnetic property through injection moulding.The results are shown in Table 4.
Table 3
NXT102,g NdFeB,g Polyvinyl alcohol, g The PPS resin, g
Embodiment 4 100 20000 100.5 1608
Embodiment 5 100 20000 402 1608
Embodiment 6 100 20000 402 2412
Embodiment 7 400 20000 102 1632
Embodiment 8 400 20000 102 2448
Embodiment 9 400 20000 408 1632
Embodiment 10 400 20000 408 2004
Embodiment 11 200 20000 202 1616
The magnetic property of table 4 NdFeB/PPS composite material
Br,Gs Hcb,Oe Hcj,Oe (BH)max,MGOe
Embodiment 4 5250 4350 8960 5.92
Embodiment 5 5150 4330 8950 5.85
Embodiment 6 4990 4130 8860 5.13
Embodiment 7 5170 4230 8940 5.88
Embodiment 8 5030 4140 8980 5.18
Embodiment 9 5210 4320 8990 5.89
Embodiment 10 4980 4110 8930 5.11
Embodiment 11 5310 4420 8960 5.98

Claims (5)

1. the preparation method of a NdFeB/PPS injection moulding particle material is characterized in that the preparation method carries out as follows:
(1) coupling processing: 0.5~2 mass parts coupling agent is dissolved with alcohol, add 100 mass parts NdFeB magnetics then, the consumption of alcohol is enough to soak into the NdFeB magnetic, mixing, then 40~60 ℃ of following intensive dryings, grind broken, screening, obtain coupling NdFeB magnetic, described coupling agent is a titante coupling agent;
(2) pre-granulation: get coupling NdFeB magnetic 100 mass parts that step (1) makes, the polyvinyl alcohol of 0.5~2 mass parts is dissolved in the deionized water, form clear solution, in described clear solution, add the Powdered PPS resin of the coupling NdFeB magnetic of getting and 8~12 mass parts, mix, 70~90 ℃ of following intensive dryings, cooling is taken out grinding and is broken into particulate material then;
(3) mixing, the pelletizing acquisition NdFeB/PPS injection moulding particle material of the particulate material that step (2) is obtained.
2. the preparation method of NdFeB/PPS injection moulding particle material as claimed in claim 1 is characterized in that described coupling agent is NXT102.
3. the preparation method of NdFeB/PPS injection moulding particle material as claimed in claim 1 is characterized in that described NdFeB magnetic prepares by quick quenching technique or HDDR method.
4. the preparation method of NdFeB/PPS injection moulding particle material as claimed in claim 1 is characterized in that described alcohol is absolute ethyl alcohol.
5. the preparation method of NdFeB/PPS injection moulding particle material as claimed in claim 1 is characterized in that described method carries out according to following steps:
The NdFeB magnetic that quick quenching technique is obtained carries out coupling processing: with the coupling agent anhydrous alcohol solution of 0.5~2 mass parts, the fast quenching NdFeB magnetic that adds 100 mass parts, the amount of absolute ethyl alcohol is just soaked the NdFeB magnetic, under ventilation condition, constantly stir, fully mix magnetic and coupling agent, then 40~60 ℃ of following intensive dryings, being cooled to room temperature takes out, grind broken, screening, obtain coupling fast quenching NdFeB magnetic, described coupling agent is NXT102;
Pre-granulation is handled: the polyvinyl alcohol of 0.5~2 mass parts is dissolved in forms colourless transparent solution in the deionized water, the Powdered PPS resin that adds 100 mass parts coupling fast quenching NdFeB magnetics and 8~12 mass parts again, constantly stir simultaneously, magnetic, PPS resin are mixed with polyvinyl alcohol evenly, 70~90 ℃ of following intensive dryings are cooled to room temperature taking-up grinding and are broken into the particulate material that particle diameter is not more than 5mm;
The particulate material that obtains is mixing, pelletizing obtains the NdFeB/PPS injection moulding particle material.
CN200710067880A 2007-04-06 2007-04-06 Method for preparing NdFeB/PPS injection moulding particle material Expired - Fee Related CN100593828C (en)

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US20140377915A1 (en) * 2013-06-20 2014-12-25 Infineon Technologies Ag Pre-mold for a magnet semiconductor assembly group and method of producing the same

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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
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