CN106433085B - A kind of technology of preparing of the neodymium iron boron of high filler loading capacity-poly (arylene ether nitrile) composite sheet - Google Patents
A kind of technology of preparing of the neodymium iron boron of high filler loading capacity-poly (arylene ether nitrile) composite sheet Download PDFInfo
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- CN106433085B CN106433085B CN201610807925.6A CN201610807925A CN106433085B CN 106433085 B CN106433085 B CN 106433085B CN 201610807925 A CN201610807925 A CN 201610807925A CN 106433085 B CN106433085 B CN 106433085B
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- 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
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- 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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Abstract
The present invention relates to a kind of neodymium iron boron of high filler loading capacity-poly (arylene ether nitrile) composite sheet preparation methods, belong to technical field of polymer materials.The system prepares neodymium iron boron-poly (arylene ether nitrile) composite material of high filler loading capacity by the method that casting film-forming and hot press forming technology combine, the composite material exhibits go out high thermal decomposition temperature (>=450 DEG C) and preferably mechanical strength (24.70-78.09MPa), the composite functional material is expected to meet the application requirement of the industries such as electronic equipment, motor, can further widen neodymium iron boron-poly (arylene ether nitrile) composite material application field.
Description
Technical field
The present invention relates to a kind of neodymium iron boron of high filler loading capacity-poly (arylene ether nitrile) composite sheet technologies of preparing, including the system
Casting film-forming, hot-forming preparation method, belong to technical field of polymer materials under specific process conditions.Gained height is filled out
The neodymium iron boron composite material of charge has the characteristics that high magnetic, high temperature resistant and abrasion-resistant.
Background technique
Nd-Fe-B permanent magnet since the advent of the world, since it has many advantages, such as high energy product, high-coercive force and small in size, 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 for electricity
Machine, can substantially reduced motor weight and volume, improve motor performance and reach energy-saving and environment-friendly effect.It is bored with the aluminium nickel of early stage
Motor is bored with rare earth to compare, although the introducing of neodymium iron boron alleviates the weight and volume of motor, pursues the electricity of more lighting
Machine and reduction production cost are that the following Nd-Fe-B permanent-magnet motor becomes to what lighting, high-performance and inexpensive direction were developed
Gesture.Meanwhile the low defects such as low with operating temperature of antioxygenic property of neodymium iron boron are also to hinder the key of its further development and application
Therefore problem improves its inoxidizability and temperature tolerance is also one of emphasis research topic.
Poly aromatic ether nitrile high molecular polymer has thermo-oxidative stability outstanding, corrosion resistant as a kind of special polymer material
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 many advantages, such as high specific strength, good thermal insulation, flexibility and the molding of light and easy processing, can make
It is structure and function profile material in numerous areas such as aerospace, machine-building, electronic equipment, auto industry and electromechanics trades
It is used widely.
In conclusion neodymium iron boron inorganic particulate is added in poly aromatic ether nitrile high molecular polymer, polyarylether may be implemented
Nitrile high molecular polymer to effective cladding of neodymium iron boron inorganic particulate, improve its inoxidizability, temperature tolerance and have it is light and
The features such as easy processing；Meanwhile the neodymium iron boron composite material of high filler loading capacity is still able to maintain its excellent magnetic property.Therefore, in conjunction with poly-
The excellent characteristics of aryl oxide nitrile high molecular and neodymium iron boron is expected to develop a kind of high-content, high temperature resistant, corrosion-resistant, anti-oxidant and have
There is neodymium iron boron-poly (arylene ether nitrile) composite sheet of good flexibility, light weight and easy processing molding, is expected in aviation
Space flight, electronic equipment, machine-building and electromechanics trade etc. are used widely.
Summary of the invention
The object of the present invention is to provide a kind of preparations of the neodymium iron boron with high inorganic content-poly (arylene ether nitrile) composite sheet
Method.It is molten that the present invention by the neodymium iron boron inorganic fill particle of high-content, by ultrasonic agitation is dispersed in a kind of poly (arylene ether nitrile)
In liquid, a kind of neodymium iron boron-poly (arylene ether nitrile) compound system is obtained；Then, casting film-forming under the conditions of graded temperature-control, is prepared neodymium
Iron boron-poly (arylene ether nitrile) laminated film；Finally, hot-forming under certain temperature and pressure condition, it is prepared with high-content
Neodymium iron boron-poly (arylene ether nitrile) composite sheet.Poly (arylene ether nitrile) composite sheet preparation provided by the present invention with high inorganic content
It is simple process, at low cost, it is advantageously implemented the large-scale production of neodymium iron boron-poly (arylene ether nitrile) composite material.
A kind of preparation method of the neodymium iron boron with high inorganic content-poly (arylene ether nitrile) composite sheet, feature exist
In:
1, neodymium iron boron-poly (arylene ether nitrile) laminated film preparation, by the poly (arylene ether nitrile) solution of the content of different neodymium iron borons through super
Casting filming therapy is used after sound dispersion, the solvent in film is removed under the conditions of graded temperature-control, the neodymium iron boron-for preparing high-content is poly-
Aryl oxide nitrile laminated film；
2, the neodymium iron boron of different structure-poly (arylene ether nitrile) laminated film preparation, by adjusting the knot of poly aromatic ether nitrile high molecular
Structure obtains neodymium iron boron-poly (arylene ether nitrile) laminated film of different structure；
3, neodymium iron boron-poly (arylene ether nitrile) composite sheet preparation, under certain temperature and pressure, answering as described in feature 1 and 2
Film is closed by hot-forming, neodymium iron boron-poly (arylene ether nitrile) composite sheet is prepared；
4, 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 is bought from market, 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.
5, the neodymium iron boron inorganic particulate as described in feature 4, partial size≤5 μm；
6, the content of neodymium iron boron is 40-70% in composite material as described in feature 1；
7, the preparation of laminated film is that poly aromatic ether nitrile high molecular is dissolved in N, N- by casting filming therapy as described in feature 1
It is formed in dimethylformamide (NMP) solvent, poly aromatic ether nitrile high molecular and NMP are mixed by the matter liquor ratio of 1:10；
8, graded temperature-control method, temperature program(me) as described in feature 1 are as follows: 80 DEG C of -1h, 100 DEG C of -1h, 120 DEG C of -1h, 160 DEG C -
2h,200℃-2h；
9, the structural formula of different structure poly (arylene ether nitrile) is shown below as described in feature 2
Bisphenol A-type
Biphenyl type
P-phenyl
10, as described in feature 3, hot-forming temperature is 260-320 DEG C, pressure 10-20MPa, hot pressing time 1-
4h。
11, neodymium iron boron-poly (arylene ether nitrile) composite sheet wearability test: Taber5750 Linear wear-resistant tester is used；It surveys
Strip part: load 500N, movement speed are 60 back and forth/minute, moving distance 2.0, standard bistrique using H-18 bistrique,
Testing time 10 minutes, finally with the wearability of Volume erosion rate characterization sheet material.
Beneficial effects of the present invention: neodymium iron boron-poly (arylene ether nitrile) composite material of high inorganic content provided by the present invention
Preparation method is simple, low in cost；Using poly (arylene ether nitrile) as organic carrier, it is coated on neodymium iron boron surface, can effectively prevent its oxygen
Change, improve the inoxidizability of composite board, at the same the correlated performance test result of composite material can satisfy its electronic equipment,
Neodymium iron boron-poly (arylene ether nitrile) composite material application field has further been widened in the application of the industries such as motor.
Detailed description of the invention:
The scanning electron microscopic picture of neodymium iron boron described in Fig. 1
The structure of bisphenol A-type, biphenyl type described in Fig. 2 and p-phenyl's poly aromatic ether nitrile high molecular
Specific embodiment:
The embodiment of preparation method of the present invention introduced below, but following embodiment is for illustrating of the invention show
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 by step (1),
By 3h is stirred by ultrasonic, keeps neodymium iron boron inorganic particulate evenly dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Neodymium is prepared in step (1) obtained compound system casting film-forming under the conditions of graded temperature-control by step (2)
Iron boron-poly (arylene ether nitrile) laminated film, graded temperature-control program be 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 step (2) obtained laminated film, is prepared neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
Manufactured composite sheet through the above steps, performance test: tensile strength 78.09MPa, elasticity modulus
3531.62MPa, thermal decomposition temperature are 450 DEG C, Volume erosion rate 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 by step (1),
By 3h is stirred by ultrasonic, keeps neodymium iron boron inorganic particulate evenly dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Neodymium iron is prepared in step (1) obtained compound system casting film-forming under the conditions of graded temperature-control by step (2)
Boron-poly (arylene ether nitrile) laminated film, graded temperature-control program be 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 step (2) obtained laminated film, is prepared neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
Manufactured composite sheet through the above steps, performance test: tensile strength 63.63MPa, elasticity modulus
4424.39MPa, thermal decomposition temperature are 455 DEG C, Volume erosion rate 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 by step (1),
By 3h is stirred by ultrasonic, keeps neodymium iron boron inorganic particulate evenly dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Neodymium iron is prepared in step (1) obtained compound system casting film-forming under the conditions of graded temperature-control by step (2)
Boron-poly (arylene ether nitrile) laminated film, graded temperature-control program be 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 step (2) obtained laminated film, is prepared neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
Manufactured composite sheet through the above steps, performance test: tensile strength 61.49MPa, elasticity modulus
4878.97MPa, thermal decomposition temperature are 460 DEG C, Volume erosion rate 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 by step (1),
By 3h is stirred by ultrasonic, keeps neodymium iron boron inorganic particulate evenly dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Neodymium iron is prepared in step (1) obtained compound system casting film-forming under the conditions of graded temperature-control by step (2)
Boron-poly (arylene ether nitrile) laminated film, graded temperature-control program be 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 step (2) obtained laminated film, is prepared neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
Manufactured composite sheet through the above steps, performance test: tensile strength 25.70MPa, elasticity modulus
5820.37MPa, thermal decomposition temperature are 478 DEG C, Volume erosion rate 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 by step (1),
By 3h is stirred by ultrasonic, keeps neodymium iron boron inorganic particulate evenly dispersed in the solution, obtain neodymium iron boron-poly (arylene ether nitrile) compound system；
Neodymium iron is prepared in step (1) obtained compound system casting film-forming under the conditions of graded temperature-control by step (2)
Boron-poly (arylene ether nitrile) laminated film, graded temperature-control program be 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 step (2) obtained laminated film, is prepared neodymium
Iron boron-poly (arylene ether nitrile) composite sheet；
Manufactured composite sheet through the above steps, performance test: tensile strength 24.70MPa, elasticity modulus
5620.37MPa, thermal decomposition temperature are 520 DEG C, Volume erosion rate 13%.
Claims (8)
1. a kind of neodymium iron boron-poly (arylene ether nitrile) laminated film preparation method, which is characterized in that the neodymium iron boron of different content is inorganic
Particle is added in the solution of poly aromatic ether nitrile high molecular, is stirred by ultrasonic, and keeps neodymium iron boron inorganic particulate evenly dispersed in the solution,
Obtain neodymium iron boron-poly (arylene ether nitrile) compound system；Casting film-forming under the conditions of graded temperature-control, removes the solvent in film, and preparation is high
The neodymium iron boron of content-poly (arylene ether nitrile) laminated film；
The neodymium iron boron inorganic particulate, partial size≤5 μm；
The content of neodymium iron boron inorganic particulate is 40-70% in laminated film.
2. a kind of preparation method of neodymium iron boron-poly (arylene ether nitrile) laminated film according to claim 1, which is characterized in that logical
The structure for crossing adjustment poly aromatic ether nitrile high molecular, obtains neodymium iron boron-poly (arylene ether nitrile) laminated film of different structure.
3. neodymium iron boron-the poly (arylene ether nitrile) being prepared by the neodymium iron boron in claim any one of 1-2-poly (arylene ether nitrile) laminated film
Composite sheet, which is characterized in that under certain temperature and pressure, the neodymium iron boron-poly (arylene ether nitrile) laminated film is passed through into hot pressing
Molding, is prepared neodymium iron boron-poly (arylene ether nitrile) composite sheet.
4. a kind of -2 described in any item neodymium iron boron-poly (arylene ether nitrile) preparation method of composite film, feature exist according to claim 1
In the laminated film is made of neodymium iron boron inorganic particulate, poly aromatic ether nitrile high molecular；Neodymium iron boron inorganic particulate is purchased from market
It buys, poly aromatic ether nitrile high molecular is bisphenol A-type, biphenyl type and p-phenyl's poly aromatic ether nitrile high molecular, is prepared by laboratory.
5. a kind of preparation method of neodymium iron boron-poly (arylene ether nitrile) laminated film according to claim 1, which is characterized in that institute
Casting film-forming is stated, concrete operations are to be dissolved in poly aromatic ether nitrile high molecular in n,N-Dimethylformamide (NMP) solvent being formed,
Wherein poly aromatic ether nitrile high molecular and NMP are mixed by the matter liquor ratio of 1:10.
6. a kind of preparation method of neodymium iron boron-poly (arylene ether nitrile) laminated film according to claim 1, which is characterized in that institute
State graded temperature-control method, temperature program(me) are as follows: 80 DEG C of -2h, 100 DEG C of -2h, 120 DEG C of -1h, 160 DEG C of -1h, 200 DEG C of -2h.
7. a kind of preparation method of neodymium iron boron-poly (arylene ether nitrile) laminated film according to claim 2, which is characterized in that institute
The structural formula for stating poly aromatic ether nitrile high molecular is shown below:
8. a kind of neodymium iron boron according to claim 3-poly (arylene ether nitrile) laminated film sheet material preparation method, described to be hot pressed into
The temperature of type is 260-320 DEG C, pressure 10-20MPa, hot pressing time 1-4h.
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Citations (2)
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7390579B2 (en) * | 2003-11-25 | 2008-06-24 | Magnequench, Inc. | Coating formulation and application of organic passivation layer onto iron-based rare earth powders |
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Patent Citations (2)
| 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 |
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