CN109912969A - A kind of fiberglass reinforced PA 66 composite material and preparation method - Google Patents
A kind of fiberglass reinforced PA 66 composite material and preparation method Download PDFInfo
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- CN109912969A CN109912969A CN201910055252.7A CN201910055252A CN109912969A CN 109912969 A CN109912969 A CN 109912969A CN 201910055252 A CN201910055252 A CN 201910055252A CN 109912969 A CN109912969 A CN 109912969A
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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
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/06—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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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Abstract
The invention discloses a kind of fiberglass reinforced PA 66 composite materials, are formulated by weight percentage by the raw material of following proportion, PA 66 PA66:55-65%；Nucleating agent: 1-3%；Long glass fibres: 32-35%；Antioxidant: 0.1-0.3%；Coupling agent: 0.1-0.2%.The specific advantage for the fiberglass reinforced PA 66 composite material that the present invention obtained obtain is as follows: the present invention effectively raises the mechanical strength of composite material；The present invention effectively shortens the molding cycle of composite material；The present invention solves the problems, such as stomata of the thick-wall part in forming process；Material of the present invention is mainly used in railway fastener system, such as rail fastening, rail insulation backing plate, the products such as track gauge block, service sleeve and apron block.
Description
Technical field
The present invention relates to a kind of technical field of polymer materials, especially a kind of fiberglass reinforced PA 66 is compound
Material and preparation method.
Background technique
Fiberglass reinforced PA 66 composite material, specific strength are higher than common metal, and metal parts is compared, light,
Antirust, antivibration, shock resistance, creep resistant is good, and dimensional stability is higher, has the small advantage of specific gravity concurrently, can be for a long time in high temperature and humidity
In the environment of work.Based on the above advantage, fiberglass reinforced PA 66 composite material be widely used in automobile, furniture,
The fields such as building, tool.Recently as the development of high-speed railway, it is multiple to use a large amount of fiberglass reinforced PA 66
Condensation material, such as railway apron block, rail insulation track gauge block and railroad sleeper casing.Fiberglass reinforced PA 66 is compound
Material has been widely applied in the tracks fastener such as casing, track gauge block, apron block, shake when can solve locomotive operation,
Noise problem, and be able to maintain wheelbase and stablize, it is possible to reduce maintenance frequency, good vibration resistance, to ensure high-speed rail it is steady very
It is important.In order to ensure the safety and long-term effect of sleeper cannula system, China Academy of Railways Sciences increase selected glass
The mechanical property of strong nylon material has higher requirements, and wherein tensile strength is not less than 150MPa, and bending strength is not less than 200MPa,
Unnotched impact strength is not less than 80KJ/m 2, and glass mass fraction is 30%-35%.Therefore need to research and develop a novel glass
Fiber enhanced nylon material meets above-mentioned requirements.
Summary of the invention
There is provided the purpose of the present invention is to solve above-mentioned the deficiencies in the prior art a kind of fiberglass reinforced polyadipate oneself
Diamines composite material and preparation method, the fiberglass reinforced PA 66 composite material have good mechanical performance, especially
It is tensile strength, bending strength and impact strength, heat resistance, and good molding processibility is very suitable for as high-speed railway
Fastener uses.
To achieve the goals above, a kind of fiberglass reinforced PA 66 composite material designed by the present invention, by
The raw material matched below are formulated by weight percentage,
PA 66 PA66:55-65%；Nucleating agent: 1-3%；Long glass fibres: 32-35%；Antioxidant:
0.1-0.3%；Coupling agent: 0.1-0.2%.
Wherein the PA 66 PA66 is the pure PA 66 resin of viscosity 2.4-3.2,
The antioxidant is N, N'- is bis--(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, three [2.4-
Di-tert-butyl-phenyl] phosphite ester,
The diameter of the long glass fibres is 8-15 microns,
The coupling agent is silane coupling agent,
The nucleating agent is the mixture of the one or both of polyamide PA46, TP1401.
A kind of preparation method of fiberglass reinforced PA 66 composite material, comprising the following steps:
Step 1: according to PA 66 PA66:55-65%；Nucleating agent: 1-3%；Long glass fibres: 32-
35%；Antioxidant: 0.1-0.3%；Coupling agent: the weight ratio of 0.1-0.2% carries out weighing raw material；
Step 2: it is mixed after PA 66 PA66, coupling agent, nucleating agent, antioxidant are mixed in order in bipyramid
It is mixed 10-15 minutes in glassware, revolving speed is at 10-20 revs/min；
Step 3: being placed in melting extrusion in double screw extruder for the raw material mixed, is granulated, while in extrusion process
Long glass fibres is added from the middle section glass fiber opening position of extruder, processing technology is 275-285 DEG C of an area, two area 265-275
DEG C, three 255-265 DEG C of areas, four 245-255 DEG C of areas, five 235-245 DEG C of areas；
Step 4: it is finally that the complete particle of above-mentioned granulation is 4-6 hours dry in 120 DEG C of air dry oven, then exist
It is formed in injector.
It is used in the present invention using polyamide PA46 and TP1401 as nucleating agent, polyamide PA46 and TP1401 have good
Thermal stability, crystallization rate is fast at high temperature, and crystalline core size is tiny and uniform, can effectively improve the type of polyamide PA66
Can, shorten the molding cycle of polyamide PA66, processes under hot conditions and stablize and do not allow volatile, while product is with higher
Glossiness.The addition of coupling agent can be even closer by the interface cohesion of glass and polyamide PA66 simultaneously, is conducive to mechanical performance
Promotion.
The specific advantage for the fiberglass reinforced PA 66 composite material that the present invention obtained obtain is as follows: the present invention
Effectively raise the mechanical strength of composite material；The present invention effectively shortens the molding cycle of composite material；The present invention solves
Stomata problem of the thick-wall part in forming process；Material of the present invention is mainly used in railway fastener system, as rail is buckled
Part, rail insulation backing plate, the products such as track gauge block, service sleeve and apron block.
Specific embodiment
Below with reference to embodiment, the present invention is further described.
In following embodiment and comparative example, PA 66 is the viscosity 2.4-3.2 of producers such as refreshing horse, Rhodia
Pure resin.Nucleating agent is Royal DSM PA46, Brueggemann TP1401.Toughener Du Pont maleic anhydride grafted ethene octene copolymer
N493D.Antioxidant is N, N'- is bis--(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, three [the tertiary fourths of 2.4- bis-
Base phenyl] phosphite ester (commercially available 1098,168 etc.).Coupling agent is one of commercially available KH550, KH560.The long glass used
Fibre diameter is 8-15 microns (main manufacturer is megalith, day another name for Sichuan Province, Mount Taishan etc.).
Embodiment 1 (following example content of raw material is weight percentage)
It is mixed in bipyramid blender after PA66 65.2, coupling agent 0.3, nucleating agent 1, antioxidant 0.5 are mixed in order
10-15 minutes, revolving speed was granulated at 30-60/ minutes, then through melting extrusion in double screw extruder, while adding roving glass fiber 33.
Its processing technology is 275-285 DEG C of an area, 265-275 DEG C of 2nd area, three 255-265 DEG C of areas, four 245-255 DEG C of areas, five area 235-
245℃。
Embodiment 2 (following example content of raw material is weight percentage)
It is mixed in bipyramid blender after PA66 64.7, coupling agent 0.2, nucleating agent 1.5, antioxidant 0.5 are mixed in order
It closes 10-15 minutes, revolving speed is granulated at 30-60/ minutes, then through melting extrusion in double screw extruder, while adding roving glass fiber
33.Its processing technology is 275-285 DEG C of an area, 265-275 DEG C of 2nd area, three 255-265 DEG C of areas, four 245-255 DEG C of areas, 5th area
235-245℃。
Embodiment 3
It is mixed in bipyramid blender after PA66 62.2, coupling agent 0.2, nucleating agent 3, antioxidant 0.5 are mixed in order
10-15 minutes, revolving speed was granulated at 30-60/ minutes, then through melting extrusion in double screw extruder, while adding roving glass fiber 33.
Its processing technology is 275-285 DEG C of an area, 265-275 DEG C of 2nd area, three 255-265 DEG C of areas, four 245-255 DEG C of areas, five area 235-
245℃。
Embodiment 4
It is mixed in bipyramid blender after PA6661.2, coupling agent 0.2, nucleating agent 4, antioxidant 0.5 are mixed in order
10-15 minutes, revolving speed was granulated at 30-60/ minutes, then through melting extrusion in double screw extruder, while adding roving glass fiber 33.
Its processing technology is 275-285 DEG C of an area, 265-275 DEG C of 2nd area, three 255-265 DEG C of areas, four 245-255 DEG C of areas, five area 235-
245℃。
Embodiment 5
It is mixed in bipyramid blender after PA66 60.2, coupling agent 0.2, nucleating agent 5, antioxidant 0.5 are mixed in order
10-15 minutes, revolving speed was granulated at 30-60/ minutes, then through melting extrusion in double screw extruder, while adding roving glass fiber 33.
Its processing technology is 275-285 DEG C of an area, 265-275 DEG C of 2nd area, three 255-265 DEG C of areas, four 245-255 DEG C of areas, five area 235-
245℃。
Comparative example 1
It is mixed 10-15 minutes in bipyramid blender after PA66, coupling agent, antioxidant are mixed in order, revolving speed is in 30-
60/ minute, then through melting extrusion in double screw extruder, be granulated, while adding roving glass fiber 33.Its processing technology is an area 275-
285 DEG C, 265-275 DEG C of 2nd area, three 255-265 DEG C of areas, four 245-255 DEG C of areas, five 235-245 DEG C of areas.
Comparative example 2
10-15 is mixed in bipyramid blender after PA66, coupling agent, nucleating agent, toughener, antioxidant are mixed in order
Minute, revolving speed is granulated at 30-60/ minutes, then through melting extrusion in double screw extruder, while adding roving glass fiber 33.It is processed
Technique is 275-285 DEG C of an area, 265-275 DEG C of 2nd area, three 255-265 DEG C of areas, four 245-255 DEG C of areas, five 235-245 DEG C of areas.
Comparative example 3
It mixes 10-15 minutes, turns in bipyramid blender after PA66, coupling agent, toughener, antioxidant are mixed in order
Speed is granulated at 30-60/ minutes, then through melting extrusion in double screw extruder, while adding roving glass fiber 33.Its processing technology is
One 275-285 DEG C of area, 265-275 DEG C of 2nd area, three 255-265 DEG C of areas, four 245-255 DEG C of areas, five 235-245 DEG C of areas.
The complete particle of above-mentioned granulation is 4-6 hours dry in 120 DEG C of air dry oven, then carried out in injector
The molding of test bars.
Tensile property is tested according to ISO 527-2, and specimen size is 150mm × 10mm × 4mm, and tensile speed is
5mm/min, bending property are tested according to ISO 178, and specimen size is 80mm × 10mm × 4mm, test speed 2mm/
Min, span 64mm, the non-notch impact strength of simply supported beam are tested according to ISO 179 (1eU), specimen size be 80mm ×
10mm × 4mm, mobility are tested according to ISO 1133, and test condition is 280 DEG C, counterweight 2.16kg.
The intensity of composite material carries out overall merit by tensile strength, bending strength and impact strength.
From embodiment 1-3 as can be seen that with the increase for being nucleated agent content, roving glass fiber diameter becomes smaller, composite material
Mechanical strength and non-notch impact strength all at apparent increased trend.Embodiment 4-5 does not become in fixed glass diameter
In the case of, the content of simple increase nucleating agent, performance declines, but straight using thick glass relative to embodiment 1-2
In the case where diameter, mechanical performance and non-notched impact properties improve, but the performance gap relative to embodiment 3 is bright
It is aobvious.In nucleating agent, coupling agent and the suitable situation of antioxidant additive amount, the comprehensive performance highest of embodiment 3 is especially non-lacks
The suitable of 4% toughener is added in the impact strength and comparative example of mouth, while other mechanical performances will be higher by very much, Injection moulded part
Appearance it is good, molding cycle is obviously shortened, and the spherocrystal that polyamide material is formed in forming process at this time is of moderate size, and by
In the presence of coupling agent, the interface cohesion of spherocrystal and glass is close, and mechanical performance is optimal.When nucleation dosage is less, polyamide material
Expect that the spherocrystal formed is larger, the interface cohesion of spherocrystal and glass is loose；When nucleation agent content is more, the ball of polyamide material formation
Brilliant too small, the interface cohesion that will also result in spherocrystal and glass is loose, either way will cause the comprehensive mechanical of composite material
The reduction of energy.The additive amount of suitable glass diameter and nucleating agent is selected, the cost of composite material can not only be significantly reduced,
Enough mechanical performances can also be provided simultaneously for composite material.
Claims (7)
1. a kind of fiberglass reinforced PA 66 composite material, it is characterised in that: by following proportion raw material by weight
Percentage is formulated, PA 66 PA66:55-65%；Nucleating agent: 1-3%；Long glass fibres: 32-35%；Antioxygen
Agent: 0.1-0.3%；Coupling agent: 0.1-0.2%.
2. a kind of fiberglass reinforced PA 66 composite material according to claim 1, it is characterised in that: described poly-
Hexamethylene diamine adipate PA66 is the pure PA 66 resin of viscosity 2.4-3.2.
3. a kind of fiberglass reinforced PA 66 composite material according to claim 1, it is characterised in that: described anti-
Oxygen agent is N, N'- is bis--(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, three [2.4- di-tert-butyl-phenyls]
Phosphite ester.
4. a kind of fiberglass reinforced PA 66 composite material according to claim 1, it is characterised in that: the length
The diameter of glass fibre is 8-15 microns.
5. a kind of fiberglass reinforced PA 66 composite material according to claim 1, it is characterised in that: the idol
Connection agent is silane coupling agent.
6. a kind of fiberglass reinforced PA 66 composite material according to claim 1, it is characterised in that: it is described at
Core agent is the mixture of the one or both of polyamide PA46, TP1401.
7. a kind of preparation method of the fiberglass reinforced PA 66 composite material as described in claim 1-6, including with
Lower step:
Step 1: according to PA 66 PA66:55-65%；Nucleating agent: 1-3%；Long glass fibres: 32-35%；Antioxygen
Agent: 0.1-0.3%；Coupling agent: the weight ratio of 0.1-0.2% carries out weighing raw material；
Step 2: in bipyramid blender after PA 66 PA66, coupling agent, nucleating agent, antioxidant are mixed in order
Middle mixing 10-15 minutes, revolving speed is at 10-20 revs/min；
Step 3: being placed in melting extrusion in double screw extruder for the raw material mixed, is granulated, while from crowded in extrusion process
Out machine middle section glass fiber opening position be added long glass fibres, processing technology be 275-285 DEG C of an area, 265-275 DEG C of 2nd area, three
255-265 DEG C of area, four 245-255 DEG C of areas, five 235-245 DEG C of areas；
Step 4: it is finally that the complete particle of above-mentioned granulation is 4-6 hours dry in 120 DEG C of air dry oven, then injecting
It is formed on machine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910055252.7A CN109912969A (en) | 2019-01-21 | 2019-01-21 | A kind of fiberglass reinforced PA 66 composite material and preparation method |
| CN202111104916.8A CN113736251A (en) | 2019-01-21 | 2019-01-21 | Glass fiber reinforced polyhexamethylene adipamide composite material and preparation method thereof |
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| CN110746772A (en) * | 2019-10-21 | 2020-02-04 | 中山海明中科新材料有限公司 | Modified nylon 66 material and preparation method and application thereof |
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