CN104513479A - Preparation method of PA6 nano-composite material with magnetic property - Google Patents
Preparation method of PA6 nano-composite material with magnetic property Download PDFInfo
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- CN104513479A CN104513479A CN201410794566.6A CN201410794566A CN104513479A CN 104513479 A CN104513479 A CN 104513479A CN 201410794566 A CN201410794566 A CN 201410794566A CN 104513479 A CN104513479 A CN 104513479A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a preparation method of a PA6 nano-composite material with a magnetic property. The preparation method comprises the following steps: uniformly mixing the following raw materials in parts by weight: 10-20 parts of PA6, 75-85 parts of nanometer magnetic powder, 1-3 parts of a flexibilizer, 0.1-0.3 part of an antioxidant, 1-3 parts of nanometer powder, and 0.5-2 parts of a coupling agent, then carrying out melt extrusion, and finally pelletizing to obtain the product. According to the formula system, a magnetic core can be obtained by an injection molding manner; the properties of the magnetic core are not lower than that of the conventional die-cast molded magnetic core; the defects that the die-cast formation speed is low and discontinuous can be overcome.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic property PA6 nano composite material.
Background technology
The soft magnetic materials of resin base magnetic composite, has excellent soft magnetic performance, with low cost, is soft magnetic materials field novel material with strongest influence power, along with the development in science and technology of making rapid progress, requires also to improve constantly to soft magnetic performance.Particularly workability, more needs to improve.
Nylon is the general designation of polymeric amide, is the extrusion resin that in five large general engineering plastic, output is maximum, kind is maximum, most widely used, over-all properties is the most excellent.In polyamide resin, output and the consumption of nylon 6 and nylon66 fiber are maximum, account for about 90% of total polymeric amide, and nylon mainly has outstanding feature in mechanics, chemistry, thermal property etc.
Generally need the compression moulding of soft magnetism powder now more, nano-magnetic powder is made powder core through colloidal sol-coated-impregnation-compression moulding.The defect of compression moulding is: process speed is slow, and discontinuous.
Summary of the invention
The object of the invention is to a kind of preparation method of magnetic property PA6 nano composite material.
The technical solution used in the present invention is:
A preparation method for magnetic property PA6 nano composite material, it is made up of the raw material of following mass parts: the oxidation inhibitor of the nano-magnetic powder of PA6,75-85 part of 10-20 part, the toughner of 1-3 part, 0.1-0.3 part, the nano-powder of 1-3 part, the coupling agent of 0.5-2 part; Described nano-magnetic powder is preparation like this: by annealed for Fe73.5-Cu1-Nb3-Si13.5-Be9 amorphous band embrittlement process, argon shield ball milling becomes amorphous powder, then anneals through tubular type atmospheric resistance furnace.
Annealing Embrittlement temperature is 200-400 DEG C, and brittle time is 0.5-2 hour.
Tubular type atmospheric resistance furnace annealing 300-600 DEG C, annealing time is 1-3 hour.
Described nano-powder is preparation like this:
1) polynite is washed, sodium, pulverize;
2) fully mixed with water by the powder obtained after above-mentioned pulverizing, add acidifying with acetic acid, the system pH of making is 4.8-5.2;
3) sufficient standing, extracts upper suspension, and heating, adds Cetyltrimethylammonium bromide wherein, be fully uniformly mixed, and filters, and dries, and pulverizes.
Described toughner is at least one in ethylene methyl methacrylate multipolymer, ethylene-methyl acrylate copolymer.
Described oxidation inhibitor is at least one in Hinered phenols antioxidant, phosphite ester kind antioxidant, monothioester kind antioxidant, composite antioxidant.
Described coupling agent is at least one in silane coupling agent, titanate coupling agent, aluminate coupling agent, zirconium ester coupling agent, rare-earth coupling agent.
Described oxidation inhibitor is 1010,1076,168,264,1098,300,1024,2246,697,3114,330,412S, 626,835, at least one in B1171, B215, B225, B900, DLTP, DSTP, TNPP.
Described coupling agent is at least one in KH550, KH560, KH570, KH580, KH602, KH792, NDZ-101, NDZ-102, NDZ-105, NDZ-130, NDZ-131, NDZ-132, NDZ-133, NDZ-201, NDZ-401, NDZ-311, NDZ-311W.
The invention has the beneficial effects as follows: formula system of the present invention, the mode of injection moulding can be adopted to obtain magnetic core, and performance is not defeated by the magnetic core of traditional die cast, and it is slow to solve die cast speed, discontinuous shortcoming.
Embodiment
A preparation method for magnetic property PA6 nano composite material, it is made up of the raw material of following mass parts: the oxidation inhibitor of the nano-magnetic powder of PA6,75-85 part of 10-20 part, the toughner of 1-3 part, 0.1-0.3 part, the nano-powder of 1-3 part, the coupling agent of 0.5-2 part;
Described nano-magnetic powder is preparation like this:
1. by annealed for Fe73.5-Cu1-Nb3-Si13.5-Be9 amorphous band embrittlement process: Annealing Embrittlement temperature is 200-400 DEG C, and brittle time is 0.5-2 hour;
2. argon shield ball milling becomes 400-600 object amorphous powder, then anneals through tubular type atmospheric resistance furnace: tubular type atmospheric resistance furnace annealing 300-600 DEG C, annealing time is 1-3 hour.
Described nano-powder is preparation like this:
1) polynite is washed, sodium, pulverize;
2) be 1:(5-10 with water according to mass ratio by the powder obtained after above-mentioned pulverizing) fully mix, add acidifying with acetic acid, the system pH of making is 4.8-5.2;
3) sufficient standing, extracts upper suspension, and heating, adds Cetyltrimethylammonium bromide wherein, be fully uniformly mixed, and filters, and dries, is ground into 1000-2000 object powder.
Described toughner is at least one in ethylene methyl methacrylate multipolymer, ethylene-methyl acrylate copolymer.
Described oxidation inhibitor is at least one in Hinered phenols antioxidant, phosphite ester kind antioxidant, monothioester kind antioxidant, composite antioxidant; Preferably, described oxidation inhibitor is 1010,1076,168,264,1098,300,1024,2246,697,3114,330,412S, 626,835, at least one in B1171, B215, B225, B900, DLTP, DSTP, TNPP.
Described coupling agent is at least one in silane coupling agent, titanate coupling agent, aluminate coupling agent, zirconium ester coupling agent, rare-earth coupling agent; Preferably, described coupling agent is at least one in KH550, KH560, KH570, KH580, KH602, KH792, NDZ-101, NDZ-102, NDZ-105, NDZ-130, NDZ-131, NDZ-132, NDZ-133, NDZ-201, NDZ-401, NDZ-311, NDZ-311W.
Below in conjunction with specific embodiment, formula of the present invention is described further:
embodiment 1:
A preparation method for magnetic property PA6 nano composite material, step is as follows:
The raw material of following mass parts is mixed: the PA6 of 20 parts, the nano-magnetic powder of 75 parts, the toughner ethylene methyl methacrylate multipolymer of 2 parts, the antioxidant 1010 of 0.2 part, the irgasfos 168 of 0.1 part, the nano-powder of 2 parts, the coupling agent KH550 of 1 part; Melt extrude again, granulation.
Wherein:
Described nano-magnetic powder is preparation like this: by Fe73.5-Cu1-Nb3-Si13.5-Be9 amorphous band through 250 DEG C of Annealing Embrittlement process 2h, argon shield ball milling becomes 500 order amorphous powders, then enters tubular type atmospheric resistance furnace 500 DEG C annealing 3h.
Described nano-powder is preparation like this:
1) polynite is washed, sodium, pulverize;
2) be that 1:5 fully mix with water according to mass ratio by the powder obtained after above-mentioned pulverizing, add acidifying with acetic acid, the system pH of making is 5;
3) sufficient standing, extracts upper suspension, and heating, adds Cetyltrimethylammonium bromide wherein, be fully uniformly mixed, and filters, and dries, is ground into 1500 object powders.
embodiment 2:
A preparation method for magnetic property PA6 nano composite material, step is as follows:
The raw material of following mass parts is mixed: the PA6 of 15 parts, the nano-magnetic powder of 80 parts, the toughner ethylene methyl methacrylate multipolymer of 2 parts, the antioxidant 1010 of 0.2 part, the irgasfos 168 of 0.1 part, the nano-powder of 2 parts, the coupling agent KH550 of 1 part; Melt extrude again, granulation.
Wherein:
Described nano-magnetic powder is preparation like this: by Fe73.5-Cu1-Nb3-Si13.5-Be9 amorphous band through 250 DEG C of Annealing Embrittlement process 2h, argon shield ball milling becomes 500 order amorphous powders, then enters tubular type atmospheric resistance furnace 500 DEG C annealing 3h.
Described nano-powder is preparation like this:
1) polynite is washed, sodium, pulverize;
2) be that 1:8 fully mix with water according to mass ratio by the powder obtained after above-mentioned pulverizing, add acidifying with acetic acid, the system pH of making is 5;
3) sufficient standing, extracts upper suspension, and heating, adds Cetyltrimethylammonium bromide wherein, be fully uniformly mixed, and filters, and dries, is ground into 1500 object powders.
comparative example:
A preparation method for magnetic property matrix material, step is: by Fe73.5-Cu1-Nb3-Si13.5-Be9 amorphous band through 250 DEG C of Annealing Embrittlement process 2h, argon shield ball milling becomes 500 order amorphous powders, then enters tubular type atmospheric resistance furnace 500 DEG C annealing 3h.
Mixed by quality 1:1 with E51 epoxy resin by above-mentioned powder, stir 15min, vacuum leaves standstill 10min, then pour into matrix material through circular grinding tool.
Be magnetic core by the matrix material injection moulding of embodiment 1-2, the magnetic core made with the matrix material die cast of comparative example carries out performance test, the SY8232 type B-H analyser adopting Japan to produce carries out the test of this journey energy, elementary 300 circles of test coil, enameled wire diameter 0.31mm; Secondary coil 60 circle, enameled wire diameter 0.21mm, is placed in frequency 1000kHz, tests under the condition of magnetic field 3mT; Its result is as following table:
table 1: magnetic core performance
Can be drawn to draw a conclusion by magnetic behavior: adopt the magnetic of injection moulding can replace traditional die cast completely, solve die casting speed slow, discontinuous defect simultaneously.
Claims (9)
1. a preparation method for magnetic property PA6 nano composite material, is characterized in that: step is as follows: mixed by the raw material of following masses part: the oxidation inhibitor of the nano-magnetic powder of PA6,75-85 part of 10-20 part, the toughner of 1-3 part, 0.1-0.3 part, the nano-powder of 1-3 part, the coupling agent of 0.5-2 part; Melt extrude again, granulation;
Wherein, described nano-magnetic powder is preparation like this: by annealed for Fe73.5-Cu1-Nb3-Si13.5-Be9 amorphous band embrittlement process, argon shield ball milling becomes amorphous powder, then anneals through tubular type atmospheric resistance furnace.
2. the preparation method of a kind of magnetic property PA6 nano composite material according to claim 1, it is characterized in that: Annealing Embrittlement temperature is 200-400 DEG C, brittle time is 0.5-2 hour.
3. the preparation method of a kind of magnetic property PA6 nano composite material according to claim 1, is characterized in that: tubular type atmospheric resistance furnace annealing 300-600 DEG C, annealing time is 1-3 hour.
4. the preparation method of a kind of magnetic property PA6 nano composite material according to claim 1, is characterized in that: described nano-powder is preparation like this:
1) polynite is washed, sodium, pulverize;
2) fully mixed with water by the powder obtained after above-mentioned pulverizing, add acidifying with acetic acid, the system pH of making is 4.8-5.2;
3) sufficient standing, extracts upper suspension, and heating, adds Cetyltrimethylammonium bromide wherein, fully stirs mixed
Close, filter, dry, pulverize.
5. the preparation method of a kind of magnetic property PA6 nano composite material according to claim 1, is characterized in that: described toughner is at least one in ethylene methyl methacrylate multipolymer, ethylene-methyl acrylate copolymer.
6. the preparation method of a kind of magnetic property PA6 nano composite material according to claim 1, is characterized in that: described oxidation inhibitor is at least one in Hinered phenols antioxidant, phosphite ester kind antioxidant, monothioester kind antioxidant, composite antioxidant.
7. the preparation method of a kind of magnetic property PA6 nano composite material according to claim 1, is characterized in that: described coupling agent is at least one in silane coupling agent, titanate coupling agent, aluminate coupling agent, zirconium ester coupling agent, rare-earth coupling agent.
8. the preparation method of a kind of magnetic property PA6 nano composite material according to claim 6, is characterized in that: described oxidation inhibitor is 1010,1076,168,264,1098,300,1024,2246,697,3114,330,412S, 626,835, at least one in B1171, B215, B225, B900, DLTP, DSTP, TNPP.
9. the preparation method of a kind of magnetic property PA6 nano composite material according to claim 7, is characterized in that: described coupling agent is at least one in KH550, KH560, KH570, KH580, KH602, KH792, NDZ-101, NDZ-102, NDZ-105, NDZ-130, NDZ-131, NDZ-132, NDZ-133, NDZ-201, NDZ-401, NDZ-311, NDZ-311W.
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| CN201410794566.6A CN104513479A (en) | 2014-12-19 | 2014-12-19 | Preparation method of PA6 nano-composite material with magnetic property |
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| CN201410794566.6A CN104513479A (en) | 2014-12-19 | 2014-12-19 | Preparation method of PA6 nano-composite material with magnetic property |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07256570A (en) * | 1994-03-22 | 1995-10-09 | Aichi Steel Works Ltd | Nail gun and magnet body therefor |
| CN1855623A (en) * | 2005-04-26 | 2006-11-01 | 阿莫先思电子电器有限公司 | Absorber for radio-frequency identificating antenna and radio-frequency identificating antenna using the same |
| CN102744403A (en) * | 2012-06-19 | 2012-10-24 | 同济大学 | Preparation method of nanocrystalline magnetic powder cores |
| CN104087833A (en) * | 2014-06-18 | 2014-10-08 | 安泰科技股份有限公司 | Iron-based nanocrystalline soft-magnetic alloy with excellent high-frequency performance and preparation method thereof |
-
2014
- 2014-12-19 CN CN201410794566.6A patent/CN104513479A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07256570A (en) * | 1994-03-22 | 1995-10-09 | Aichi Steel Works Ltd | Nail gun and magnet body therefor |
| CN1855623A (en) * | 2005-04-26 | 2006-11-01 | 阿莫先思电子电器有限公司 | Absorber for radio-frequency identificating antenna and radio-frequency identificating antenna using the same |
| CN102744403A (en) * | 2012-06-19 | 2012-10-24 | 同济大学 | Preparation method of nanocrystalline magnetic powder cores |
| CN104087833A (en) * | 2014-06-18 | 2014-10-08 | 安泰科技股份有限公司 | Iron-based nanocrystalline soft-magnetic alloy with excellent high-frequency performance and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| HEE-JIN KIM ET AL.: "Effect of Binders on the Magnetic Behavior of P/M Processed FeSiBCuNb Alloy", 《MATERIALS SCIENCE FORUM VOLS 449-452》 * |
| 杨秋平: "注射成型技术制备各向异性粘结铷铁硼磁体的研究", 《万方数据企业知识服务平台》 * |
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