CN106433085A - Preparation technology of neodymium-iron-boron-polyaryl ether nitrile composite sheet with high filling volume - Google Patents
Preparation technology of neodymium-iron-boron-polyaryl ether nitrile composite sheet with high filling volume Download PDFInfo
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- CN106433085A CN106433085A CN201610807925.6A CN201610807925A CN106433085A CN 106433085 A CN106433085 A CN 106433085A CN 201610807925 A CN201610807925 A CN 201610807925A CN 106433085 A CN106433085 A CN 106433085A
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2371/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
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- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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Abstract
The invention relates to a preparation technology of a neodymium-iron-boron-polyaryl ether nitrile composite sheet with a high filling volume and belongs to the technical field of macromolecular materials. According to the system, through the combination of a film casting technology and a hot press molding technology, the neodymium-iron-boron-polyaryl ether nitrile composite material with the high filling volume is prepared, has high thermal decomposition temperature which is larger than or equal to 450 DEG C and excellent mechanical strength which ranges from 24.70 MPa to 78.09 MPa, is expected to meet the application requirements of industries such as electronic equipment and motors, and can further expand the application field.
Description
Technical field
The present invention relates to a kind of technology of preparing of the neodymium iron boron of high filler loading capacity-poly (arylene ether nitrile) composite sheet, including this system
Under specific process conditions, casting film-forming, hot-forming preparation method, belong to technical field of polymer materials.Gained height is filled out
The neodymium iron boron composite of charge has the features such as high magnetic, high temperature resistant and abrasion-resistant.
Background technology
Nd-Fe-B permanent magnet since the advent of the world, because it has the advantages that high energy product, high-coercive force and small volume, quilt
It is widely used in the fields such as electronic information, machinery, electromechanics and national defence.Wherein, as rare earth permanent-magnetic material, high-performance neodymium iron
Boron has important purposes in the motor of new-energy automobile, wind power generation and convertible frequency air-conditioner etc..Nd-Fe-B permanent magnet is used for electricity
Machine, can substantially mitigate motor weight and volume, improve motor performance and the effect reaching energy-conserving and environment-protective.Bore with the aluminium nickel of early stage
Bore motor with rare earth to compare, although the introducing of neodymium iron boron alleviates the weight and volume of motor, pursue the electricity of more lighting
Machine and reduction production cost, are following Nd-Fe-B permanent-magnet motors to becoming that lighting, high-performance and inexpensive direction are developed
Gesture.Meanwhile, the antioxygenic property of neodymium iron boron is low and the low defect of operating temperature is also to hinder the key of its further development and application
Problem, therefore, improving its non-oxidizability and temperature tolerance is also one of emphasis research topic.
Poly aromatic ether nitrile high molecular polymer, as a kind of speciality polymer material, has prominent thermo-oxidative stability, corrosion resistant
The features such as corrosion, mechanical performance and excellent anti-flammability and insulating properties.Compared with most of metal and inorganic material, polyarylether
Nitrile high molecular polymer has the advantages that high specific strength, good thermal insulation, pliability and light weight and easy processing are molded, and can make
For 26S Proteasome Structure and Function section bar material in numerous areas such as Aero-Space, machine-building, electronic equipment, auto industry and electromechanics trades
It is used widely.
In sum, neodymium iron boron inorganic particulate is added in poly aromatic ether nitrile high molecular polymer, it is possible to achieve polyarylether
Effective cladding to neodymium iron boron inorganic particulate for the nitrile high molecular polymer, improve its non-oxidizability, temperature tolerance and have light weight and
The features such as easy processing；Meanwhile, the neodymium iron boron composite of high filler loading capacity remains to keep its excellent magnetic property.Therefore, in conjunction with poly-
Aryl oxide nitrile high molecular and the excellent specific property of neodymium iron boron, are expected to develop a kind of high-load, high temperature resistant, corrosion-resistant, anti-oxidant and tool
There is neodymium iron boron-poly (arylene ether nitrile) composite sheet that good pliability, light weight and easy processing are molded, be expected in aviation
Space flight, electronic equipment, machine-building and electromechanics trade etc. are used widely.
Content of the invention
It is an object of the invention to provide a kind of preparation of the neodymium iron boron-poly (arylene ether nitrile) composite sheet with high inorganic content
Method.The present invention, by the neodymium iron boron inorganic fill particle of high-load, is dispersed in a kind of poly (arylene ether nitrile) by ultrasonic agitation molten
In liquid, obtain a kind of neodymium iron boron-poly (arylene ether nitrile) compound system；Subsequently, casting film-forming under the conditions of graded temperature-control, prepares neodymium
Iron boron-poly (arylene ether nitrile) laminated film；Finally, under uniform temperature and pressure condition, hot-forming, prepare with high-load
Neodymium iron boron-poly (arylene ether nitrile) composite sheet.The poly (arylene ether nitrile) composite sheet preparation with high inorganic content provided by the present invention
Process is simple, low cost, are advantageously implemented the large-scale production of neodymium iron boron-poly (arylene ether nitrile) composite material.
A kind of preparation method of described neodymium iron boron-poly (arylene ether nitrile) composite sheet with high inorganic content, its feature exists
In：
1st, the preparation of neodymium iron boron-poly (arylene ether nitrile) laminated film, by the poly (arylene ether nitrile) solution of the content of different neodymium iron borons through super
Adopt casting filming therapy after sound dispersion, remove the solvent in film under the conditions of graded temperature-control, prepare the neodymium iron boron of high-load-poly-
Aryl oxide nitrile laminated film；
2nd, the preparation of the neodymium iron boron of different structure-poly (arylene ether nitrile) laminated film, by adjusting the knot of poly aromatic ether nitrile high molecular
Structure, obtains the neodymium iron boron-poly (arylene ether nitrile) laminated film of different structure；
3rd, the preparation of neodymium iron boron-poly (arylene ether nitrile) composite sheet, under uniform temperature and pressure, answering as described in feature 1 and 2
Close film by hot-forming, prepare neodymium iron boron-poly (arylene ether nitrile) composite sheet；
4th, the neodymium iron boron as described in feature 1 and 2-poly (arylene ether nitrile) laminated film is high by neodymium iron boron inorganic particulate, poly (arylene ether nitrile)
Molecule is constituted.Neodymium iron boron derives from market and buys, and poly aromatic ether nitrile high molecular is bisphenol A-type, biphenyl type and p-phenyl's polyarylether
Nitrile high molecular, is prepared by laboratory.
5th, the neodymium iron boron inorganic particulate as described in feature 4, its particle diameter≤5 μm；
6th, in composite as described in feature 1, the content of neodymium iron boron is 40-70%；
7th, casting filming therapy is passed through in the preparation of laminated film as described in feature 1, is that poly aromatic ether nitrile high molecular is dissolved in N, N-
Formed in dimethylformamide (NMP) solvent, poly aromatic ether nitrile high molecular and NMP press 1:10 matter liquor ratio mixing；
8th, graded temperature-control method as described in feature 1, its temperature program(me) is：80℃-1h、100℃-1h、120℃-1h、160℃-
2h、200℃-2h；
9th, as described in feature 2, the structural formula of different structure poly (arylene ether nitrile) is shown below
Bisphenol A-type
Biphenyl type
P-phenyl
10th, as described in feature 3, hot-forming temperature is 260-320 DEG C, and pressure is 10-20MPa, and hot pressing time is 1-
4h.
11st, neodymium iron boron-poly (arylene ether nitrile) composite sheet wearability test：Using Taber5750 Linear wear-resistant tester；Survey
Strip part：Load is 500N, and translational speed is 60 back and forth/minute, displacement 2.0, and standard bistrique uses H-18 bistrique,
10 minutes testing times, finally characterize the wearability of sheet material with Volume erosion rate.
Beneficial effects of the present invention：Neodymium iron boron-the poly (arylene ether nitrile) composite material of high inorganic content provided by the present invention
Preparation method is simple, with low cost；Using poly (arylene ether nitrile) as organic carrier, it is coated on neodymium iron boron surface, can effectively stop its oxygen
Change, improve composite board non-oxidizability, simultaneously the correlated performance test result of composite can meet its electronic equipment,
The application of the industries such as motor, has widened the application of neodymium iron boron-poly (arylene ether nitrile) composite material further.
Brief description：
The scanning electron microscopic picture of neodymium iron boron described in Fig. 1
The structure of bisphenol A-type, biphenyl type and p-phenyl's poly aromatic ether nitrile high molecular described in Fig. 2
Specific embodiment：
The embodiment of preparation method of the present invention introduced below, but following embodiment is for showing of the present invention is described
Example, does not constitute any restriction to the claims in the present invention.
Embodiment 1：
40 parts of neodymium iron boron inorganic particulates are added in the solution containing 60 parts of bisphenol A-type poly aromatic ether nitrile high moleculars step (1),
Through ultrasonic agitation 3h, make neodymium iron boron inorganic particulate dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Step (2) casting film-forming under the conditions of graded temperature-control by the compound system obtained by step (1), prepares neodymium
Iron boron-poly (arylene ether nitrile) laminated film, graded temperature-control program is 80 DEG C of -2h, 100 DEG C of -2h, 120 DEG C of -1h, 160 DEG C of -1h, 200 DEG C -
2h；
Step (3) hot pressing 4h under the conditions of 260 DEG C, 15MPa by the laminated film obtained by step (2), prepares neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
The composite sheet made by above-mentioned steps, its performance test：Tensile strength 78.09MPa, elastic modelling quantity
3531.62MPa, heat decomposition temperature is 450 DEG C, and Volume erosion rate is 16%.
Embodiment 2：
50 parts of neodymium iron boron inorganic particulates are added in the solution containing 50 parts of bisphenol A-type poly aromatic ether nitrile high moleculars step (1),
Through ultrasonic agitation 3h, make neodymium iron boron inorganic particulate dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Step (2) casting film-forming under the conditions of graded temperature-control by the compound system obtained by step (1), prepares neodymium iron
Boron-poly (arylene ether nitrile) laminated film, graded temperature-control program is 80 DEG C of -2h, 100 DEG C of -2h, 120 DEG C of -1h, 160 DEG C of -1h, 200 DEG C -
2h；
Step (3) hot pressing 4h under the conditions of 280 DEG C, 15MPa by the laminated film obtained by step (2), prepares neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
The composite sheet made by above-mentioned steps, its performance test：Tensile strength 63.63MPa, elastic modelling quantity
4424.39MPa, heat decomposition temperature is 455 DEG C, and Volume erosion rate is 19%.
Case study on implementation 3
60 parts of neodymium iron boron inorganic particulates are added in the solution containing 40 parts of bisphenol A-type poly aromatic ether nitrile high moleculars step (1),
Through ultrasonic agitation 3h, make neodymium iron boron inorganic particulate dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Step (2) casting film-forming under the conditions of graded temperature-control by the compound system obtained by step (1), prepares neodymium iron
Boron-poly (arylene ether nitrile) laminated film, graded temperature-control program is 80 DEG C of -2h, 100 DEG C of -2h, 120 DEG C of -1h, 160 DEG C of -1h, 200 DEG C -
2h；
Step (3) hot pressing 4h under the conditions of 300 DEG C, 15MPa by the laminated film obtained by step (2), prepares neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
The composite sheet made by above-mentioned steps, its performance test：Tensile strength 61.49MPa, elastic modelling quantity
4878.97MPa, heat decomposition temperature is 460 DEG C, and Volume erosion rate is 15%.
Case study on implementation 4
70 parts of neodymium iron boron inorganic particulates are added in the solution containing 30 parts of bisphenol A-type poly aromatic ether nitrile high moleculars step (1),
Through ultrasonic agitation 3h, make neodymium iron boron inorganic particulate dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Step (2) casting film-forming under the conditions of graded temperature-control by the compound system obtained by step (1), prepares neodymium iron
Boron-poly (arylene ether nitrile) laminated film, graded temperature-control program is 80 DEG C of -2h, 100 DEG C of -2h, 120 DEG C of -1h, 160 DEG C of -1h, 200 DEG C -
2h；
Step (3) hot pressing 4h under the conditions of 320 DEG C, 15MPa by the laminated film obtained by step (2), prepares neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
The composite sheet made by above-mentioned steps, its performance test：Tensile strength 25.70MPa, elastic modelling quantity
5820.37MPa, heat decomposition temperature is 478 DEG C, and Volume erosion rate is 12%.
Case study on implementation 5
70 parts of neodymium iron boron inorganic particulates are added in the solution containing 30 parts of biphenyl type poly aromatic ether nitrile high moleculars step (1),
Through ultrasonic agitation 3h, make neodymium iron boron inorganic particulate dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Step (2) casting film-forming under the conditions of graded temperature-control by the compound system obtained by step (1), prepares neodymium iron
Boron-poly (arylene ether nitrile) laminated film, graded temperature-control program is 80 DEG C of -2h, 100 DEG C of -2h, 120 DEG C of -1h, 160 DEG C of -1h, 200 DEG C -
2h；
Step (3) hot pressing 4h under the conditions of 300 DEG C, 20MPa by the laminated film obtained by step (2), prepares neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
The composite sheet made by above-mentioned steps, its performance test：Tensile strength 24.70MPa, elastic modelling quantity
5620.37MPa, heat decomposition temperature is 520 DEG C, and Volume erosion rate is 13%.
Claims (10)
1. the preparation of neodymium iron boron-poly (arylene ether nitrile) laminated film, by the poly (arylene ether nitrile) solution of the content of different neodymium iron borons through ultrasonic point
Adopt casting filming therapy after dissipating, remove the solvent in film under the conditions of graded temperature-control, prepare the neodymium iron boron-polyarylether of high-load
Nitrile laminated film；
2. the preparation of the neodymium iron boron of different structure-poly (arylene ether nitrile) laminated film, by adjusting the structure of poly aromatic ether nitrile high molecular, obtains
Neodymium iron boron-poly (arylene ether nitrile) laminated film to different structure；
3. the preparation of neodymium iron boron-poly (arylene ether nitrile) composite sheet, the THIN COMPOSITE under uniform temperature and pressure, as described in feature 1 and 2
Film, by hot-forming, prepares neodymium iron boron-poly (arylene ether nitrile) composite sheet；
4. the neodymium iron boron as described in feature 1 and 2-poly (arylene ether nitrile) laminated film, by neodymium iron boron inorganic particulate, poly aromatic ether nitrile high molecular
Constitute.Neodymium iron boron derives from market and buys, and poly aromatic ether nitrile high molecular is that bisphenol A-type, biphenyl type and p-phenyl's poly (arylene ether nitrile) are high
Molecule, is prepared by laboratory.
5. the neodymium iron boron inorganic particulate as described in feature 4, its particle diameter≤5 μm；
6. in composite as described in feature 1, the content of neodymium iron boron is 40-70%；
7. casting filming therapy is passed through in the preparation of laminated film as described in feature 1, is that poly aromatic ether nitrile high molecular is dissolved in N, N- diformazan
Formed in base formamide (NMP) solvent, poly aromatic ether nitrile high molecular and NMP press 1:10 matter liquor ratio mixing；
8. graded temperature-control method as described in feature 1, its temperature program(me) is：80℃-1h、100℃-1h、120℃-1h、160℃-2h、
200℃-2h；
9. as described in feature 2, the structural formula of different structure poly (arylene ether nitrile) is shown below
Bisphenol A-type
Biphenyl type
P-phenyl
10. as described in feature 3, hot-forming temperature is 260-320 DEG C, and pressure is 10-20MPa, and hot pressing time is 1-4h.
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| CN201610807925.6A CN106433085B (en) | 2016-09-07 | 2016-09-07 | A kind of technology of preparing of the neodymium iron boron of high filler loading capacity-poly (arylene ether nitrile) composite sheet |
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| CN201610807925.6A CN106433085B (en) | 2016-09-07 | 2016-09-07 | A kind of technology of preparing of the neodymium iron boron of high filler loading capacity-poly (arylene ether nitrile) composite sheet |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030155548A1 (en) * | 2000-04-28 | 2003-08-21 | Satoshi Ozawa | Hydraulic-composition bond magnet |
| CN102775755A (en) * | 2012-07-31 | 2012-11-14 | 电子科技大学 | Polyaryl ether nitrile (PEN) and carbonyl iron powder (Fe(CO)5) composite magnetic material and preparation method thereof |
| EP2653302A2 (en) * | 2003-11-25 | 2013-10-23 | Magnequench, Inc. | Coating formulation and application of organic passivation layer onto iron-based rare earth powders |
-
2016
- 2016-09-07 CN CN201610807925.6A patent/CN106433085B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030155548A1 (en) * | 2000-04-28 | 2003-08-21 | Satoshi Ozawa | Hydraulic-composition bond magnet |
| EP2653302A2 (en) * | 2003-11-25 | 2013-10-23 | Magnequench, Inc. | Coating formulation and application of organic passivation layer onto iron-based rare earth powders |
| CN102775755A (en) * | 2012-07-31 | 2012-11-14 | 电子科技大学 | Polyaryl ether nitrile (PEN) and carbonyl iron powder (Fe(CO)5) composite magnetic material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 周存忠等: "《永磁理论与技术及其在油田中的应用》", 30 June 1994, 石油工业出版社 * |
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