CN112795178A - High-strength polyamide wave-absorbing material and preparation method and application thereof - Google Patents
High-strength polyamide wave-absorbing material and preparation method and application thereof Download PDFInfo
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2241—Titanium dioxide
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
The invention discloses a high-strength polyamide wave-absorbing material which comprises the following components in parts by weight: poly(s) are polymerized30-70 parts of amide; 5-60 parts of continuous basalt fibers; 0.1-2 parts of a flow modifier; 1-30 parts of a wave absorbing agent; 0.2-0.8 part of antioxidant; 0.1-1 part of lubricant, and drawing out the continuous basalt fiber after dipping in a dipping die head. The notch impact strength of the wave-absorbing material is more than or equal to 15kJ/m2(ii) a The lowest wave absorbing performance can play a role in the range of-10 to-29 dB.
Description
Technical Field
The invention relates to the technical field of high polymer materials, and particularly relates to a high-strength polyamide wave-absorbing material, and a preparation method and application thereof.
Background
Polyamide (PA), commonly known as nylon, is a generic name for thermoplastic resins containing recurring amide groups- [ NH-CO ] -in the molecular backbone, including aliphatic PA, aliphatic-aromatic PA and aromatic PA. The PA has excellent performances of high strength, high wear resistance, oil resistance, weak acid resistance, self lubrication, insulating processing and the like, and is widely applied to a plurality of industries such as automobiles, machinery, electric tools, traffic, buildings and the like. At present, with the development of domestic high-speed 5G networks, various Internet of things devices in various industries have higher and higher requirements on material electromagnetic performance, for example, in an intelligent automobile, some sensors need to emit waves in a specific direction and receive reflected waves from the specific direction, and shell materials of the sensors need certain wave-transmitting materials and certain wave-absorbing materials, so that misjudgment caused by receiving the waves in different directions is avoided.
Chinese patent (CN102936370A) discloses a continuous fiber reinforced thermoplastic resin prepreg tape and a preparation method thereof, wherein wave-absorbing substances are added into a system, so that the prepreg tape has wave-absorbing performance, but the prepreg tape has obvious defects, on one hand, the components of the prepreg tape and the wave-absorbing substances are not uniformly mixed, and a large amount of wave-absorbing substances are required to be added to achieve better wave-absorbing capacity, on the other hand, the prepreg tape is of a sheet structure and can only be applied in specific scenes, for example, products with simple structures such as flat plates can not be applied to some complex parts.
Disclosure of Invention
The invention provides a high-strength polyamide wave-absorbing material for overcoming the defects of insufficient wave-absorbing capacity, low strength and small application range.
The invention also aims to provide a preparation method of the high-strength polyamide wave-absorbing material.
The invention also aims to provide application of the high-strength polyamide wave-absorbing material.
In order to achieve the purpose, the invention adopts the technical scheme that:
a high-strength polyamide wave-absorbing material comprises the following components in parts by weight:
and the continuous basalt fibers are dipped in the dipping die head and then pulled out.
The flow modifier is added into the system, so that the wave absorbing agent and the continuous basalt fiber can be better dispersed, and excellent wave absorbing property can be realized by adding a small amount of the wave absorbing agent; in addition, the flow modifier can also be used as an internal lubricant between materials to prevent friction between molecules; various products with complex structures can be produced by adopting an injection molding method, and the strength and the wave-absorbing property of the polyamide resin are further improved by the mutual matching of the basalt fibers and the flow modifier, because the basalt fibers also have excellent wave-absorbing property.
The continuous basalt fiber is dipped in the dipping die head and then pulled out, so that the mechanical property of the continuous basalt fiber can be effectively prevented from being greatly reduced due to short shearing.
Preferably, the flow modifier is at least one of a low molecular weight diacid, a low molecular weight diamine, and a hyperbranched polymer containing a multi-terminal carboxyl group.
The low molecular weight dibasic acid is dibasic acid with 8-20 carbon atoms, such as dodecanedioic acid, tetradecanedioic acid and the like;
the low molecular weight diamine is diamine with 8-20 carbon atoms such as decamethylene diamine, dodecane diamine and the like
The hyperbranched polymer containing the multi-terminal carboxyl groups has the weight average molecular weight of 2000-3000 and a large number of carboxyl groups (-COOH) with strong polar functional groups on the surface.
Preferably, the wave absorbing agent is at least one of carbon black, ferrite, barium titanate, graphite, titanium dioxide, nickel powder or cobalt oxide.
Preferably, the polyamide is one or two of aliphatic polyamide and aromatic polyamide.
The aliphatic polyamide is polycaprolactam, polyhexamethylene diamine adipate and polydodecamide.
The aromatic polyamide is polyhexamethylene terephthalate or decamethylene terephthalate.
Preferably, the antioxidant is at least one of hindered phenol antioxidant, phosphite antioxidant and copper salt antioxidant.
Preferably, the antioxidant is a hindered phenol antioxidant.
The hindered phenol antioxidant is at least one of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine and other hindered phenols.
The phosphite antioxidant is at least one of bis (2, 6-di-tert-butyl-4-methylphenyl) pentaerythritol diphosphite, tris [2, 4-di-tert-butylphenyl ] phosphite and the like.
The copper salt antioxidant is a heat-resistant antioxidant containing Cu salt, and comprises organic copper salt and inorganic copper salt.
Preferably, the lubricant is at least one of an amide lubricant, a stearate lubricant, or an ester lubricant.
The invention also provides a preparation method of the high-strength polyamide wave-absorbing material, which comprises the following steps:
s1, weighing polyamide, an antioxidant, a lubricant, a proper flow modifier and a wave absorbing agent according to a proportion, and uniformly mixing to obtain a premix;
s2, adding the premix obtained in the step S1 into an extruder, carrying out melt blending, extruding into an impregnation die head, then soaking and drawing out the continuous basalt fiber in the impregnation die head, and sequentially carrying out cooling, traction and grain cutting to obtain the basalt fiber reinforced polyamide material.
Preferably, the length of the basalt fiber reinforced polyamide material is 3-25 mm.
The continuous basalt fibers in the wave-absorbing material particles are as long as the particles, and the basalt fiber reinforced PA material has better strength when the length of the basalt fiber reinforced PA material is 3-25 mm.
The high-strength polyamide wave-absorbing material is applied to preparation of anechoic chambers, microwave communication, electronic equipment and medical equipment.
Compared with the prior art, the invention has the beneficial effects that:
the invention providesThe high-strength polyamide wave-absorbing material adopts a flow modifier and basalt fiber to blend to improve the strength and wave-absorbing capacity of the wave-absorbing material, wherein the flow modifier can improve the dispersing capacity of the wave-absorbing agent and the basalt fiber, so that excellent wave-absorbing characteristics can be realized by adding a small amount of the wave-absorbing agent. The notch impact strength of the wave-absorbing material is more than or equal to 15kJ/m2(ii) a The lowest wave absorbing performance can play a role in the range of-10 to-29 dB.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, but the embodiments of the present invention are not limited thereto.
The reagents, methods and equipment adopted by the invention are conventional in the technical field if no special description is given.
The following examples and comparative examples employ the following starting materials:
polyamide: PA10T KFHP 11A: from Zhuhaiwantong;
basalt fiber: continuous basalt fiber, BC13-68 × 1 × 2-S68: from Sichuan space Tuo Xin basalt industries, Inc.;
flow modifier a: shandong HanLin biology dodecanedioic acid;
flow modifier B: decamethylenediamine Hao chemical industry;
flow modifier C: hyperbranched polymer containing multi-terminal carboxyl and Wuhan hyperbranched resin;
wave absorber A: titanium dioxide Hangzhou Dahua chemical industry;
wave absorber B: a new nickel powder Jiangsu Boqian material;
wave absorber C: ferrite Zhejiang Zhongke magnetic industry, cobalt oxide Boshan Dahe chemical industry; quality of
Wave absorber D: a graphite Qingdao Tianyuan Dai;
antioxidant: RIANOX 1098 linaloon;
lubricant: A-C540A Honeywell.
The present invention will be described in detail with reference to examples and comparative examples.
The wave-absorbing material is prepared by the following method in the embodiment and the comparative examples 1-4, and all the components are weighed according to the weight ratio in the table 1-3; the method comprises the following specific steps:
s1, weighing polyamide, an antioxidant, a lubricant, a flow modifier and a wave absorbing agent according to a proportion, and uniformly mixing to obtain a premix;
s2, adding the premix obtained in the step S1 into an extruder, carrying out melt blending, extruding into an impregnation die head, then soaking continuous basalt fibers in the impregnation die head, then drawing out, and sequentially carrying out cooling, traction and grain cutting to obtain the basalt fiber reinforced polyamide material, wherein the particle length is 3-25 mm, and the fiber and the particle in the particles are equal in length.
Examples 1 to 6
TABLE 1 formulations (parts) of examples 1 to 6
Examples 7 to 11
TABLE 2 formulations (parts) of examples 7 to 11
| Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | |
| Polyamide | 50 | 50 | 50 | 50 | 50 |
| Basalt fiber | 20 | 20 | 20 | 20 | 20 |
| Flow modifier A | 1 | 1 | 1 | 1 | 1 |
| Wave absorber A | 1 | 5 | 15 | 20 | 30 |
| Antioxidant agent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Lubricant agent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
Examples 12 to 16
TABLE 3 formulations (parts) of examples 12 to 16
| Example 12 | Example 13 | Example 14 | Example 15 | Example 16 | |
| Polyamide | 50 | 50 | 50 | 30 | 70 |
| Basalt fiber | 20 | 20 | 20 | 5 | 60 |
| Flow modifier A | 1 | 1 | 1 | 0.1 | 2 |
| Wave absorber A | — | — | — | 30 | 1 |
| Wave absorber B | 10 | — | — | — | — |
| Wave absorber C | — | 10 | — | — | — |
| Wave absorber D | — | — | 10 | — | — |
| Antioxidant agent | 0.5 | 0.5 | 0.5 | 0.8 | 0.2 |
| Lubricant agent | 0.5 | 0.5 | 0.5 | 1 | 0.1 |
Comparative examples 1 to 5
Comparative example 5 the wave-absorbing material was prepared by the following method, weighing the components in the weight ratios in table 4; the method comprises the following specific steps:
s11, weighing polyamide, an antioxidant, a lubricant, a flow modifier and a wave absorbing agent according to a proportion, and uniformly mixing to obtain a premix;
s21, adding the premix and the continuous basalt fiber obtained in the step S1 into an extruder, melting, shearing, extruding, cooling, drawing and granulating to obtain the basalt fiber reinforced polyamide material with the particle length of (4 +/-1) mm, wherein the fiber length is 0.1-0.6 mm.
TABLE 4 formulations (parts) of comparative examples 1 to 5
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
| Polyamide | 50 | 50 | 50 | 50 | 50 |
| Basalt fiber | 20 | 20 | — | — | 20 |
| Glass fiber | — | — | 20 | — | — |
| Flow modifier A | — | — | 1 | 1 | 1 |
| Wave absorber A | 10 | 40 | 10 | 10 | 10 |
| Antioxidant agent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Lubricant agent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
The properties of the high-strength wave-absorbing material obtained in each embodiment and each comparative example are detected by the following methods and standards:
1. tensile Strength determined according to ISO 527-2-2012, 5mm/min
2. The impact strength of the notch of the simply supported beam is determined according to ISO 179/1Ea-2010 at 23 DEG C
3. The frequency absorbing performance is judged according to the reflectivity, the test method is the waveguide method in GJB 5239-2004,
4. the frequency testing method comprises the following steps: the frequency and the wave-absorbing performance are obtained by testing according to GJB5329-2004 standard, the wider the frequency is, the better the coverage area is, and the higher the frequency is, the better the wave-absorbing performance is, the higher the wave-absorbing capacity of the material to electromagnetic waves is, the larger the numerical value is, the more the attenuation of the material is, and the better the wave-absorbing performance is.
TABLE 5 data for examples and comparative examples
From examples 1 to 6, the wave absorbing performance of the material gradually increases with the addition of the flow modifier.
From examples 7 to 11, the wave absorbing performance of the material gradually increases with the increase of the content of the wave absorbing agent.
In examples 12-14, different wave-absorbing materials with the same components have equivalent wave-absorbing performance and mechanical property.
According to comparative examples 1-5, the wave-absorbing performance of the material is greatly reduced without adding a flow modifier; compared with basalt fiber materials, the wave-absorbing performance of the material is greatly reduced, and the strength is also reduced. The mechanical property and the wave-absorbing property of the material are greatly reduced without adding fiber materials. From the data of comparative example 2, it can be seen that if the flow modifier is not added, the improvement of the wave absorption performance is weak due to the addition of a large amount of wave absorber, and the mechanical performance is reduced due to the addition of a large amount of wave absorber. In the comparative example 5, the selected continuous basalt fiber is not pulled out through a dipping die, so that the mechanical property is greatly reduced and the requirement cannot be met.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The high-strength polyamide wave-absorbing material is characterized by comprising the following components in parts by weight:
and the continuous basalt fibers are dipped in the dipping die head and then pulled out.
2. The high-strength polyamide wave-absorbing material of claim 1, wherein the flow modifier is at least one of a low molecular weight diacid, a low molecular weight diamine, and a hyperbranched polymer containing multi-terminal carboxyl groups.
3. The high-strength polyamide wave-absorbing material of claim 1, wherein the wave-absorbing agent is at least one of carbon black, ferrite, barium titanate, graphite, titanium dioxide, nickel powder or cobalt oxide.
4. The high-strength polyamide wave-absorbing material of claim 1, wherein the polyamide is one or both of aliphatic polyamide and aromatic polyamide.
5. The high-strength polyamide wave-absorbing material of claim 1, wherein the antioxidant is at least one of hindered phenol antioxidants, phosphite antioxidants, and copper salt antioxidants.
6. The high-strength polyamide wave-absorbing material of claim 1, wherein the antioxidant is a hindered phenol antioxidant.
7. The high-strength polyamide wave-absorbing material of claim 1, wherein the lubricant is at least one of an amide lubricant, a stearate lubricant, or an ester lubricant.
8. The preparation method of the high-strength polyamide wave-absorbing material according to any one of claims 1 to 7, which is characterized by comprising the following steps:
s1, weighing polyamide, an antioxidant, a lubricant, a flow modifier and a wave absorbing agent according to a proportion, and uniformly mixing to obtain a premix;
s2, adding the premix obtained in the step S1 into an extruder, carrying out melt blending, extruding into an impregnation die head, then soaking and pulling out the continuous basalt fiber in the impregnation die head, and sequentially carrying out cooling, traction and grain cutting to obtain the high-strength polyamide wave-absorbing material.
9. The preparation method of the high-strength polyamide wave-absorbing material according to claim 8, wherein the length of the high-strength polyamide wave-absorbing material is 3-25 mm.
10. The high-strength polyamide wave-absorbing material of any one of claims 1 to 7 is applied to the preparation of anechoic chambers, microwave communication, electronic equipment and medical equipment.
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Cited By (3)
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| CN113429779A (en) * | 2021-07-12 | 2021-09-24 | 横店集团得邦工程塑料有限公司 | Reinforced and toughened blending modified PA6/MXD6 composite material and preparation method thereof |
| CN113736359A (en) * | 2021-09-03 | 2021-12-03 | 上海唯美德科科技有限公司 | Radio frequency anti-aging conductive skin material and preparation method thereof |
| CN113801396A (en) * | 2021-08-16 | 2021-12-17 | 无锡敬仁电子材料科技有限公司 | White foamed polymer wave-absorbing material and preparation method thereof |
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| CN113736359A (en) * | 2021-09-03 | 2021-12-03 | 上海唯美德科科技有限公司 | Radio frequency anti-aging conductive skin material and preparation method thereof |
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Application publication date: 20210514 |