CN108219451A - A kind of high-content glass fiber enhanced nylon 66 composite material and preparation method - Google Patents
A kind of high-content glass fiber enhanced nylon 66 composite material and preparation method Download PDFInfo
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- CN108219451A CN108219451A CN201611149148.7A CN201611149148A CN108219451A CN 108219451 A CN108219451 A CN 108219451A CN 201611149148 A CN201611149148 A CN 201611149148A CN 108219451 A CN108219451 A CN 108219451A
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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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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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
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Abstract
The present invention relates to a kind of high-content glass fiber enhanced nylon 66 composite material and preparation methods, belong to polymeric material field.The composite material includes the component of following mass percentage content, nylon66 fiber：31.9 38%, alkali-free glass fiber：58 62%, compatilizer：2 5%, primary antioxidant：0.3 0.5%, auxiliary antioxidant：0.3 0.5%, lubricant：0.5 1.0%, wherein, the surface of the alkali-free glass fiber is coated with enhancement layer, and the material of enhancement layer is carbon nanotube or Sic nanotube, and extruding pelletization is carried out using double screw extruder.Glass fiber content is higher in composite material of the present invention, improve composite material machinery performance and mechanical property, and nanotube is coated on the surface of alkali-free glass fiber, select the length and diameter of suitable glass and the molecular weight of nylon66 fiber, the compatibility of alkali-free glass fiber and nylon66 fiber is increased, overcomes the defects of being deteriorated in the past with the increase material appearance that glass fiber content is filled in nylon.
Description
Technical field
The present invention relates to a kind of high molecular materials, and in particular to a kind of high-content glass fiber enhanced nylon 66 composite material and system
Preparation Method.
Background technology
Nylon66 fiber, i.e., diamines, molecular formula are-[NH (CH to poly- two phthaleins2)6NHOC (CH2)4CO] n-, is abbreviated as
PA66 is that one of relatively early, yield maximum, most widely used kind are developed in Ju Tai amine family.Nylon66 fiber is water white transparency half hitch
Crystalline substance thermoplastic polymer containing phthalein amine functional group in macromolecular main chain, can form hydrogen bond, be a kind of polymorphous hypocrystalline
Polymer has excellent mechanical property, wear-resisting property, self-lubricating property, corrosion resistance, and molding processibility is also preferable, but
Water absorption rate is big, modulus is low, dimensional stability and electrical property are poor, and heat resistance, light resistance, low-temperature impact resistance, dyeability also have
It waits to improve, so as to limit the scope of application of nylon66 fiber.In order to expand the scope of application of nylon66 fiber, usually nylon66 fiber is carried out
Enhancing is modified.
Fiber nylon composite material is made of reinforced phase glass, matrix phase nylon and their interphase (interface phase),
Reinforced phase mainly plays carrying, and matrix mutually mainly plays link enhancement phase and posting, and interface is that reinforced phase is connected with matrix
The bridge connect, while play stress transfer.When by load, cracked in the weakness of composite material, and pass through
The effect at interface, by the stress transfer that matrix is born to fiber, due to glass transfers, stress is spread rapidly, is prevented
Crack growth when load accumulation reaches the intensity of fiber, causes fibrous fracture, composite material is also destroyed.Due to glass
More than big 10 times of intensity and Young's modulus ratio nylon, so the addition of glass substantially increases the energy that composite material bears external force effect
Power is increased substantially in mechanical properties such as tensile strength, the bending strengths for macroscopically showing composite material.
Therefore, the performance of glass fiber enhanced nylon composite material depends not only on reinforcing fiber and the performance of nylon matrix, and
And depend greatly on the power of interfacial adhesion.If bonding interface is bad, glass does not just play humidification, due to
Modulus between glass and nylon matrix differs greatly, and is not easy to soak between the two, and nylon matrix lacks reactive work in itself
Property functional group, it is difficult to fiber generate good chemical bond close, so its composite material interface combination is weaker.In order to fully improve
The performance of glass fiber enhanced nylon composite material should improve the compatibility, wellability and reactivity of glass and nylon matrix, existing skill
Coupling agent treatment glass surface is commonly used in art, the enhancing effect of glass is improved with this.
Invention content
In order to solve the problems in the prior art, the purpose of the present invention is to, it is proposed that a kind of mechanical property is good, and surface is without floating fibre
The high-content glass fiber enhanced nylon 66 composite material of phenomenon.
The purpose of the present invention can be realized by following technical proposal：A kind of high-content glass fiber enhanced nylon 66 composite wood
Material, which is characterized in that include the component of following mass percentage content, nylon66 fiber：31.9-38%, alkali-free glass fiber：58-62%, phase
Hold agent：2-5%, primary antioxidant：0.3-0.5%, auxiliary antioxidant：0.3-0.5%, lubricant：0.5-1.0%, wherein, the alkali-free
The surface of glass is coated with enhancement layer, and the material of enhancement layer is carbon nanotube or Sic nanotube.
The three dimension scale nanotube of alkali-free glass fiber surface homoepitaxial can increased fiber surface roughness and specific surface area,
And bridging action is formed in alkali-free glass fiber and nylon66 fiber basal body interface layer, the enhancement layer of nanoscale may be embedded in nylon66 fiber matrix
Increase the multi-scale enhancement compound system of just/interlayer toughened in middle forming layer, the interfacial bond property of composite material is improved, high
The alkali-free glass fiber of content can be preferably compatible with nylon66 fiber, accelerates the crystallization rate of nylon66 fiber, effectively improves composite material circle
Modulus of shearing, yield strength and the external force of face layer are in the transmission efficiency at nylon 66 resin matrix Yu alkali-free glass fiber interface.Simultaneously
Nanotube layer can generate layer protective layer in fiber surface, and alkali-free glass fiber surface is protected not destroyed by attack, improves composite wood
The electric insulating quality of material and environment weatherability；Carbon nanotube and the density of Sic nanotube are small, intensity, rigidity, excellent tenacity,
Therefore, the preferred carbon nanotube of the material of the surface accumulation layer of alkali-free glass fiber of the present invention and Sic nanotube, and sunk using gas phase
Area method makes carbon nanotube or Sic nanotube in alkali-free glass fiber surface oriented growth, one layer of nanometer of formation around alkali-free glass fiber
Composite material sheath.
Preferably, in above-mentioned high-content glass fiber enhanced nylon 66 composite material, the enhancing layer material accounts for alkali-free glass
Fine mass percent is 0. 3-4%；By the mass percentage content control for enhancing layer material in the range, it is because this contains
The enhancing layer material of amount can coat alkali-free glass fiber to the maximum extent, and the diameter increase degree for the alkali-free glass fiber being wrapped by will not
Influence its dispersion in nylon66 fiber matrix.
Preferably, in above-mentioned high-content glass fiber enhanced nylon 66 composite material, the length of the alkali-free glass fiber is
1.5-4.5mm, a diameter of 9-14 μm.The present invention selects alkali-free glass fiber to be modified nylon66 fiber, the tensile strength of alkali-free glass fiber
It has been substantially better than alkali glass.Theoretically alkali-free glass fiber diameter is thinner, and length is longer, and enhancing effect is better, but reaches a certain and face
During boundary's point, enhancing effect does not increase counter subtract.If glass diameter is too thin, easily by screw rod shearing into fine-powder, so as to lose glass
Humidification.It is just poor with the cementability of nylon66 fiber if glass diameter is too thick, reduce the mechanical property of product.Therefore, the present invention will
The length and diameter of alkali-free glass fiber is controlled in above range, can not only be ensured the enhancing effect of alkali-free glass fiber, can also be improved nothing
Compatibility between alkali glass and nylon66 fiber.
Preferably, in above-mentioned high-content glass fiber enhanced nylon 66 composite material, the molecular weight of the nylon66 fiber is
17000-19000.Nylon66 fiber is controlled into the range of the high molecular weight nylon, which is because, in the molecular weight ranges
66 strand is longer, and branch is more, and the active end group content of nylon66 fiber increases, and increases the accessible area of nylon66 fiber, increases
The strong intermolecular force of nylon66 fiber and alkali-free glass fiber, the more conducively contact with the surface coated nanotube of alkali-free glass fiber, from
And the wellability of nylon66 fiber and alkali-free glass fiber is improved, be conducive to alkali-free glass fiber disperses in nylon66 fiber matrix, promotes nylon66 fiber pair
The cladding of alkali-free glass fiber.Within this range, molecular weight distribution is narrower, and performance is more stable.The present invention is coated with carbon using surface
The nylon66 fiber of the alkali-free glass fiber and above-mentioned molecular weight of nanotube or Sic nanotube so that during alkali-free glass fiber content 58-62%
It remains to preferably compatible with nylon66 fiber, keeps preferable appearance, and significantly improve the mechanical property of final composite material.
Preferably, in above-mentioned high-content glass fiber enhanced nylon 66 composite material, the primary antioxidant is antioxidant
1076th, one or more groups in antioxidant 1098, antioxidant 1010, antioxidant 2246, antioxidant 4010 or antioxidant DNP
It closes.
Preferably, in above-mentioned high-content glass fiber enhanced nylon 66 composite material, the auxiliary antioxidant is antioxidant
168 or the combination of one or both of antioxidant 626.
Present invention compounding addition primary antioxidant, auxiliary anti-oxidant, the two combine the thermo-oxidative ageing for significantly improving composite material
Can, process is tested in extrusion, injection and alcoholysis better aging protection is provided for material.
Preferably, in above-mentioned high-content glass fiber enhanced nylon 66 composite material, the lubricant is calcium stearate, silicon
One or more combinations of ketone, TAF or pentaerythrite stearate.
Further preferably, the lubricant is TAF.TAF has what can be combined with glass surface portion polar group
Polar group structure, in glass fiber enhanced nylon 66 compound system, TAF forms class between glass and matrix resin nylon66 fiber
Like anchoring node, the bond state of glass and matrix resin nylon66 fiber is improved, and then improve glass, inorganic filler in matrix
Dispersibility in resin.Meanwhile the lubrication property of TAF can improve the processing fluidity of composite material, further improve compound
Material
The invention also discloses a kind of preparation method of above-mentioned high-content glass fiber enhanced nylon 66 composite material, the preparation sides
Method includes the following steps：
Nylon66 fiber, compatilizer, primary antioxidant, auxiliary antioxidant and lubricant are added to high speed batch mixing by above-mentioned mass percent
It is uniformly mixed in machine, uniformly mixed material is added to double screw extruder main feeding hopper, alkali-free glass fiber is added to double spiral shells
Bar squeezes out pusher side feeding hopper, extruding pelletization, you can obtain glass fiber enhanced nylon 66 composite material.
Wherein, the rotating speed of high speed mixer is 300-380rpm/min, incorporation time 3-8min.
The engine speed of the double screw extruder is 22-30HZ, and main feeding hopper rotating speed is 10-15HZ, and side feeding hopper turns
Speed is 8-11HZ, and extrusion temperature is 295-315 DEG C.
The present invention, using the screw combinations of weak shearing, adjusts twin-screw according to glass fiber content and nylon66 fiber relative molecular weight
The rotating speed of extruder realizes best shear effect, alkali-free glass fiber is made to be uniformly dispersed in nylon66 fiber matrix, so as to obtain performance
The composite material of stable homogeneous.Meanwhile the present invention selects suitable blending extrusion temperature, and nylon66 fiber matrix is enable fully to coat
Outside alkali-free glass fiber, floating fine phenomenon is reduced, makes that final product surface is smooth, and brittleness is small.
Compared with prior art, the present invention has coated nanotube, and select suitable glass on the surface of alkali-free glass fiber
The molecular weight of length and diameter and nylon66 fiber increases the compatibility between alkali-free glass fiber and nylon66 fiber, reduces floating fine phenomenon,
Overcome the defects of being deteriorated in the past with the increase material appearance that glass fiber content is filled in nylon.And glass in composite material of the present invention
Fine content is higher, improves composite material machinery performance, especially significantly improves the wear-resisting, corrosion-resistant, anti-tired of composite material
Labor intensity and thermal stability, and molding shrinkage is reduced, the composite material of the present invention is allow to be used safely in automobile, machinery, change
The fields such as work, the high heat-resisting strong stress members of manufacture, such as automobile pressure regulation pond, air inlet manifold, throttle valve body radiator groove,
The parts such as fan blade shield.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention is further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1
High-content glass fiber enhanced nylon 66 composite material in the present embodiment includes the component of following mass percentage content, nylon
66 ：31.9%, alkali-free glass fiber：62%, compatilizer：5%, primary antioxidant 1076：0.3%, auxiliary antioxidant 168：0.3%, lubricant
Calcium stearate：0.5%, wherein, the surface of alkali-free glass fiber is coated with 0.3% carbon nanotube enhancement layer, and the length of alkali-free glass fiber is
1.5-2.0mm, a diameter of 9-11 μm, the molecular weight of nylon66 fiber is 17000-17500；
Above-mentioned nylon66 fiber, compatilizer, primary antioxidant, auxiliary antioxidant and lubricant are added in high speed mixer and mixed
Even, the rotating speed of high speed mixer is 350rpm/min, mixes and material is added to double screw extruder main feeding hopper after 5min, together
When alkali-free glass fiber is added to twin-screw extrusion pusher side feeding hopper, extruding pelletization, you can obtain glass fiber enhanced nylon 66 composite wood
Material.Wherein, the engine speed of double screw extruder is 22HZ, and main feeding hopper rotating speed is l0HZ, and side feeding hopper rotating speed is 8HZ, is squeezed
It is 295 DEG C to go out temperature.
Embodiment 2
High-content glass fiber enhanced nylon 66 composite material in the present embodiment includes the component of following mass percentage content, nylon
66 ：32%, alkali-free glass fiber：61.5%, compatilizer：4.8%, primary antioxidant 1098：0.4%, auxiliary antioxidant 168：0.4%, lubrication
Agent silicone：0.9%, wherein, the surface of alkali-free glass fiber is coated with 1.0% carbon nanotube enhancement layer, and the length of alkali-free glass fiber is 2-
2.5mm, a diameter of 10-11 μm, the molecular weight of nylon66 fiber is 17300-17700；
Above-mentioned nylon66 fiber, compatilizer, primary antioxidant, auxiliary antioxidant and lubricant are added in high speed mixer and mixed
Even, the rotating speed of high speed mixer is 320rpm/min, mixes and material is added to double screw extruder main feeding hopper after 6min, together
When alkali-free glass fiber is added to twin-screw extrusion pusher side feeding hopper, extruding pelletization, you can obtain glass fiber enhanced nylon 66 composite wood
Material.Wherein, the engine speed of double screw extruder is 23HZ, and main feeding hopper rotating speed is l1HZ, and side feeding hopper rotating speed is 8.5HZ,
Extrusion temperature is 299 DEG C.
Embodiment 3
High-content glass fiber enhanced nylon 66 composite material in the present embodiment includes the component of following mass percentage content, nylon
66 ：33%, alkali-free glass fiber：61%, compatilizer：4.5%, primary antioxidant 1010：0.3%, auxiliary antioxidant 168：0.4%, lubricant
TAF：0.8%, wherein, the surface of alkali-free glass fiber is coated with 2% carbon nanotube enhancement layer, and the length of alkali-free glass fiber is 2.5-
3.0mm, a diameter of 10-12 μm, the molecular weight of nylon66 fiber is 17500-18000；
Above-mentioned nylon66 fiber, compatilizer, primary antioxidant, auxiliary antioxidant and lubricant are added in high speed mixer and mixed
Even, the rotating speed of high speed mixer is 360rpm/min, mixes and material is added to double screw extruder main feeding hopper after 7min, together
When alkali-free glass fiber is added to twin-screw extrusion pusher side feeding hopper, extruding pelletization, you can obtain glass fiber enhanced nylon 66 composite wood
Material.Wherein, the engine speed of double screw extruder is 24HZ, and main feeding hopper rotating speed is l2HZ, and side feeding hopper rotating speed is 9HZ, is squeezed
It is 303 DEG C to go out temperature.
To the glass fiber enhanced nylon 66 composite material uniform sampling in embodiment 1-3, ISO test specimens are made with injection molding machine
Item carries out properties test to material according to mechanical property requirements.Wherein, tensile strength and elongation at break are in V=5mm/
It is tested under conditions of min according to the method for ISO527, notch impact strength is under conditions of 23 DEG C according to ISO179/leA
Method tested, bending strength and bending modulus under conditions of V=2mm/min, S=64mm according to the method for ISO178 into
Row test, hot endowmentization handle under conditions of 140 DEG C the variation of progress mechanical property after 1000h using constant temperature ageing oven.
By the mechanical property of glass fiber enhanced nylon 66 composite material and the glass of different content in 1-3 of the embodiment of the present invention
The mechanical property of reinforced PA66 composite material is compared, and (PA66+20GF represents 20% to comparison result in table 1 as shown in table 1
The glass fiber enhanced nylon 66 composite material of content, PA66+30GF represent the glass fiber enhanced nylon 66 composite material of 30% content,
PA66+40GF represents the glass fiber enhanced nylon 66 composite material of 40% content).
Table 1：The glass fiber enhanced nylon 66 of glass fiber enhanced nylon 66 composite material and different content in embodiment 1-3 is compound
The comparison of the mechanical property of material
In conclusion the glass fiber enhanced nylon 66 composite material of the present invention and the glass fiber enhanced nylon 66 composite material of different content
It compares, has in mechanical property and significantly improve, and by observing appearance its appearance smoother, without floating fine existing
As.
Specific embodiment described herein is only an example for the spirit of the invention.Technology belonging to the present invention is led
The technical staff in domain can do various modifications or additions to described specific embodiment or replace in a similar way
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (8)
1. a kind of high-content glass fiber enhanced nylon 66 composite material, which is characterized in that the composite material includes following quality
The component of degree：Nylon66 fiber：31.9-38%, alkali-free glass fiber：58-62%, compatilizer：2-5%, primary antioxidant：0.3-
0.5%, auxiliary antioxidant：0.3-0.5%, lubricant：0.5-1.0%, wherein, the surface of the alkali-free glass fiber is coated with enhancement layer,
The material of enhancement layer is carbon nanotube or Sic nanotube.
2. according to a kind of high-content glass fiber enhanced nylon 66 composite material according to claim 1, which is characterized in that described
The mass percent that enhancing layer material accounts for alkali-free glass fiber is 0.3-4%.
A kind of 3. high-content glass fiber enhanced nylon 66 composite material described in claim 1, which is characterized in that the alkali-free glass fiber
Length for 1.5-4.5mm, a diameter of 9-14 μm.
A kind of 4. high-content glass fiber enhanced nylon 66 composite material according to claim 1, which is characterized in that the nylon
66 molecular weight is 17000-19000.
5. a kind of high-content glass fiber enhanced nylon 66 composite material according to claim 1, which is characterized in that the master resists
Oxygen agent is one in antioxidant 1076, antioxidant 1098, antioxidant 1010, antioxidant 2246, antioxidant 4010, antioxidant DNP
Kind is a variety of.
A kind of 6. high-content glass fiber enhanced nylon 66 composite material according to claim 1, which is characterized in that the auxiliary
Antioxidant is one or both of irgasfos 168, antioxidant 626.
A kind of 7. high-content glass fiber enhanced nylon 66 composite material according to claim 1, which is characterized in that the lubrication
Agent is calcium stearate, one or more in silicone, TAF, pentaerythrite stearate.
8. a kind of preparation side of the high-content glass fiber enhanced nylon 66 composite material as described in claim 1-7 any claims
Method, which is characterized in that the preparation method includes the following steps：
By above-mentioned nylon66 fiber, compatilizer, primary antioxidant, auxiliary antioxidant and lubricant by claim 1 in the quality hundred
Divide than being uniformly mixed, be then added to double screw extruder main feeding hopper, alkali-free glass fiber is added to twin-screw extrusion pusher side feeds
Hopper, extruding pelletization, you can obtain glass fiber enhanced nylon 66 composite material, the engine speed of the double screw extruder is 22-
30HZ, main feeding hopper rotating speed are 10-15HZ, and side feeding hopper rotating speed is 8-11HZ, and extrusion temperature is 295-315 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233271A (en) * | 2018-09-25 | 2019-01-18 | 福建锦江科技有限公司 | Utilize the short glass fiber reinforced nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production |
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| CN104448813A (en) * | 2014-11-25 | 2015-03-25 | 浙江俊尔新材料股份有限公司 | Glass fiber reinforced polyamide 66 composite material, and preparation method and application thereof |
| CN105131592A (en) * | 2015-08-31 | 2015-12-09 | 宁波海雨新材料科技有限公司 | High-content glass fiber reinforced polyamide 66 composite material and preparing method |
| CN105131593A (en) * | 2015-08-31 | 2015-12-09 | 宁波海雨新材料科技有限公司 | High-strength high-modulus glass fiber reinforced nylon 66 composite material and preparing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104448813A (en) * | 2014-11-25 | 2015-03-25 | 浙江俊尔新材料股份有限公司 | Glass fiber reinforced polyamide 66 composite material, and preparation method and application thereof |
| CN105131592A (en) * | 2015-08-31 | 2015-12-09 | 宁波海雨新材料科技有限公司 | High-content glass fiber reinforced polyamide 66 composite material and preparing method |
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Application publication date: 20180629 |