CN113292848A - Hydrolysis-resistant glass fiber reinforced polyamide composite material and preparation method thereof - Google Patents
Hydrolysis-resistant glass fiber reinforced polyamide composite material and preparation method thereof Download PDFInfo
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- 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 hydrolysis-resistant glass fiber reinforced polyamide composite material which is prepared from the following components in parts by weight: 30-80 parts of polyamide resin, 0.5-1.0 part of dispersing agent, 3-10 parts of toughening agent, 0.05-0.2 part of initiator, 0.1-0.2 part of nucleating agent, 10-50 parts of modified glass fiber and 0.2-0.4 part of antioxidant; wherein, the modified glass fiber is glass fiber with the outer surface coated with glycidyl methacrylate (G l yc dy l methacrylate, GMA). The invention also discloses a preparation method of the hydrolysis-resistant glass fiber reinforced polyamide composite material. The glass fiber modified by GMA is used, so that the mechanical property of the polyamide composite material and the mechanical property retention rate after high-temperature water boiling are improved, and meanwhile, due to the addition of the GMA, the degradation tendency caused by hydrolysis of amido bonds in a polyamide molecular chain can be effectively avoided, and the melt strength and the mechanical property are ensured. The preparation method of the invention is simple and has no pollution.
Description
Technical Field
The invention belongs to the field of polyamide composite materials, and particularly relates to a hydrolysis-resistant glass fiber reinforced polyamide composite material and a preparation method thereof.
Background
The polyamide has good comprehensive properties including mechanical property, heat resistance, wear resistance, chemical resistance and self-lubricity, has low friction coefficient and certain flame retardance, is easy to process, is suitable for being filled with glass fibers and other fillers to enhance modification, improves the performance and expands the application range, but the polyamide molecular chain has acylamino which is easy to hydrolyze at high temperature in the process of twin-screw extrusion to decompose into amino and carboxylic acid groups, so that the molecular chain is broken, and the material strength and the performance are reduced. How to avoid polyamide hydrolysis is the key to improve the performance of polyamide materials and expand the application field of the polyamide materials.
Disclosure of Invention
In view of the defects of the prior art, the first object of the invention is to provide a hydrolysis-resistant glass fiber reinforced polyamide composite material which has the characteristics of hydrolysis resistance, high strength and high performance retention rate after water absorption.
The second purpose of the invention is to provide a preparation method of the hydrolysis-resistant glass fiber reinforced polyamide composite material, which is simple and pollution-free.
The first purpose of the invention can be achieved by adopting the following technical scheme:
the hydrolysis-resistant glass fiber reinforced polyamide composite material is characterized by being prepared from the following components in parts by weight: 30-80 parts of polyamide resin, 0.5-1.0 part of dispersing agent, 3-10 parts of toughening agent, 0.05-0.2 part of initiator, 0.1-0.2 part of nucleating agent, 10-50 parts of modified glass fiber and 0.2-0.4 part of antioxidant; wherein the modified glass fiber is glass fiber with the outer surface coated with Glycidyl Methacrylate (GMA).
Preferably, the glass fiber is alkali-free continuous glass fiber with the diameter of 10-17 microns.
Preferably, the preparation method of the modified glass fiber comprises the following steps:
a device preparation step: providing modification equipment, wherein the modification equipment comprises a pipeline, and a spraying device and a drying device are sequentially arranged in the pipeline along the glass fiber conveying direction;
spraying: sending the glass fiber into a pipeline, and spraying GMA on the outer surface of the glass fiber through a spraying device when the glass fiber moves to the position of the spraying device, so that the GMA uniformly coats the surface of the glass fiber;
and (3) drying: and after the spraying step is finished, continuously conveying the glass fibers, and drying the glass fibers by using a drying device when the glass fibers move to the position of the drying device to obtain the modified glass fibers.
Preferably, in the drying step, the drying temperature is 130-150 ℃, and the drying distance is 0.5-1.0 m.
Preferably, the antioxidant is one or more of antioxidant 168, antioxidant 626, antioxidant 1098, antioxidant 1010 and antioxidant 1076.
Preferably, the polyamide resin is a polyamide resin having a relative viscosity of 2.5 to 3.0.
Preferably, the dispersant is hyperbranched resin, and the toughening agent is one or more of POE-g-MAH, SEBS-g-MAH, EMA and EBA; the initiator is di-tert-butyl peroxide, and the nucleating agent is long carbon chain (C18-C28) carboxylate.
The second purpose of the invention can be achieved by adopting the following technical scheme:
the preparation method of the hydrolysis-resistant glass fiber reinforced polyamide composite material is characterized by comprising the following steps:
mixing: drying polyamide resin, mixing the dried polyamide resin, a dispersing agent, a toughening agent, an initiator, nucleation and an antioxidant in a high-speed mixer according to a formula ratio, and fully stirring and uniformly dispersing to obtain a mixed material;
an extrusion step: adding the mixed material into a double-screw extruder from a feed inlet of the double-screw extruder, adding the modified glass fiber with the formula amount into the double-screw extruder from an exhaust port of the double-screw extruder, and performing melt extrusion to obtain an extruded material;
and (3) pelletizing: and (4) bracing, cooling, air-drying, granulating and mixing the extruded materials.
Preferably, after the granulating step is completed, the method further comprises the steps of strong magnetism treatment and stirring homogenization treatment.
Preferably, in the mixing step, the drying temperature of the polyamide resin is 110 ℃, the drying time is 4h, the mixing temperature is normal temperature, and the mixing speed is 200-300 r/min; in the extrusion step, the length-diameter ratio of the twin-screw extruder is 48/1; the melt extrusion temperature is 200-260 ℃, and the screw rotating speed is 300-500 r/m.
The invention has the beneficial effects that:
according to the invention, Glycidyl Methacrylate (GMA) is mainly added, epoxy active functional groups in the GMA can be used as a chain extender, degraded amide groups react with terminal amino groups or terminal carboxyl groups in molecular chains through the active epoxy functional groups, and two molecular chains are reconnected to form a section, so that the molecular chain length is increased, the viscosity is increased, the mechanical property is improved, and the performance retention rate is high after water absorption. Compared with the common glass fiber, the glass fiber modified by GMA is more favorable for improving the mechanical property of the polyamide composite material and the property retention rate after high-temperature water boiling, and simultaneously, the addition of the GMA can effectively avoid the degradation of a polyamide molecular chain, the reduction of the molecular weight, the improvement of melt index and the guarantee of melt strength and mechanical property. The preparation method of the invention is simple and has no pollution.
Detailed Description
The present invention will be further described with reference to specific embodiments, and the raw materials used in the following examples are commercially available unless otherwise specified.
The hydrolysis-resistant glass fiber reinforced polyamide composite material is prepared from the following components in parts by weight: 30-80 parts of polyamide resin, 0.5-1.0 part of dispersing agent, 3-10 parts of toughening agent, 0.05-0.2 part of initiator, 0.1-0.2 part of nucleating agent, 10-50 parts of modified glass fiber and 0.2-0.4 part of antioxidant; wherein the modified glass fiber is glass fiber with the outer surface coated with Glycidyl Methacrylate (GMA).
In a preferred embodiment, the glass fiber is alkali-free continuous glass fiber with the diameter of 10-17 microns.
As a preferred embodiment, the preparation method of the modified glass fiber comprises the following steps:
a device preparation step: providing modification equipment, wherein the modification equipment comprises a pipeline, and a spraying device and a drying device are sequentially arranged in the pipeline along the glass fiber conveying direction;
spraying: sending the glass fiber into a pipeline, and spraying GMA on the outer surface of the glass fiber through a spraying device when the glass fiber moves to the position of the spraying device, so that the GMA uniformly coats the surface of the glass fiber;
and (3) drying: and after the spraying step is finished, continuously conveying the glass fibers, and drying the glass fibers by using a drying device when the glass fibers move to the position of the drying device to obtain the modified glass fibers.
In a preferred embodiment, in the drying step, the drying temperature is 130-150 ℃, and the drying distance is 0.5-1.0 m.
In a preferred embodiment, the antioxidant is one or a mixture of more than two of antioxidant 168, antioxidant 626, antioxidant 1098, antioxidant 1010 and antioxidant 1076.
As a preferable embodiment, the polyamide resin is a polyamide resin having a relative viscosity of 2.5 to 3.0, and specifically, polyamide resins such as PA6, PA66, PA56, and PPA can be used.
As a preferred embodiment, the dispersant is a hyperbranched resin, and specifically, the dispersant may be C181 resin of wuhan hyperbranched resin technologies ltd.
In a preferred embodiment, the toughening agent is one or more of POE-g-MAH, SEBS-g-MAH, EMA and EBA.
As a preferred embodiment, the initiator is di-tert-butyl peroxide, and specifically, the initiator can adopt Craine TFB117, CAV102 and Braguemann P32.
As a preferred embodiment, the nucleating agent is a long carbon chain (C18-C28) carboxylic acid salt.
A preparation method of a hydrolysis-resistant glass fiber reinforced polyamide composite material comprises the following steps:
mixing: drying polyamide resin, mixing the dried polyamide resin, a dispersing agent, a toughening agent, an initiator, nucleation and an antioxidant in a high-speed mixer according to a formula ratio, and fully stirring and uniformly dispersing to obtain a mixed material;
an extrusion step: adding the mixed material into a double-screw extruder from a feed inlet of the double-screw extruder, adding the modified glass fiber with the formula amount into the double-screw extruder from an exhaust port of the double-screw extruder, and performing melt extrusion to obtain an extruded material;
and (3) pelletizing: and (4) bracing, cooling, air-drying, granulating and mixing the extruded materials.
In a preferred embodiment, after the granulating step is completed, the method further comprises the steps of strong magnetism and stirring and homogenizing treatment.
In a preferred embodiment, in the mixing step, the drying temperature of the polyamide resin is 110 ℃, the drying time is 4h, the mixing temperature is normal temperature, and the mixing speed is 200-300 r/min; in the extrusion step, the length-diameter ratio of the twin-screw extruder is 48/1; the melt extrusion temperature is 200-260 ℃, and the screw rotating speed is 300-500 r/m.
The following are preferred embodiments of the invention:
examples 1 to 6:
the hydrolysis-resistant glass fiber reinforced polyamide composite material is prepared from the following components in parts by weight: polyamide resin, a dispersing agent, a toughening agent, an initiator, a nucleating agent, modified glass fiber and an antioxidant; wherein the modified glass fiber is glass fiber with the outer surface coated with Glycidyl Methacrylate (GMA). The specific amounts (weight ratio) of the components are shown in Table 1
TABLE 1
In examples 1 to 6, the polyamide resin was PA6, which had a relative viscosity of 2.8. The dispersant is C181 resin of Wuhan super-branched resin science and technology Limited. The initiator is di-tert-butyl peroxide (DTBP). The toughening agent is POE-g-MAH. The nucleating agent is colain TFB 117. The antioxidant is a compound antioxidant of the antioxidant 168 and the antioxidant 1098, and the weight ratio of the antioxidant 168 to the antioxidant 1098 is 1: 1. The glass fiber was a 635B glass fiber manufactured by Taishan glass fiber Co., Ltd, and had a diameter of 13 μm.
In the above embodiments 1 to 6, the preparation method of the modified glass fiber includes the following steps:
a device preparation step: providing modification equipment, wherein the modification equipment comprises a pipeline, and a spraying device and a drying device are sequentially arranged in the pipeline along the glass fiber conveying direction;
spraying: sending the glass fiber into a pipeline, and spraying GMA on the outer surface of the glass fiber through a spraying device when the glass fiber moves to the position of the spraying device, so that the GMA uniformly coats the surface of the glass fiber;
and (3) drying: and after the spraying step is finished, continuously conveying the glass fiber, and when the glass fiber is moved to the position of a drying device, drying the glass fiber by the drying device at the drying temperature of 130-150 ℃ for 0.5-1.0 m to obtain the modified glass fiber.
The preparation method of the hydrolysis-resistant glass fiber reinforced polyamide composite material of the above embodiments 1 to 6 includes:
mixing: drying the polyamide resin at the drying temperature of 110 ℃ for 4 h; mixing the dried polyamide resin, the dispersing agent, the toughening agent, the initiator, the nucleating agent and the antioxidant in a high-speed mixer according to the formula ratio, and fully stirring and uniformly dispersing to obtain a mixed material;
an extrusion step: adding the mixed material into a double-screw extruder from a feed inlet of the double-screw extruder, adding the modified glass fiber with the formula amount into the double-screw extruder from an exhaust port of the double-screw extruder, and performing melt extrusion to obtain an extruded material; the length to diameter ratio of the twin screw extruder 48/1; the melt extrusion temperature is 200-260 ℃, and the screw rotating speed is 300-500 r/m;
and (3) pelletizing: and cooling, air drying, granulating and strong magnetic treatment are carried out on the extruded materials, thus obtaining the material.
Comparative examples 1 to 5:
the glass fiber reinforced polyamide composite material of comparative examples 1 to 5 is prepared from the following components in parts by weight: polyamide resin, a dispersing agent, a toughening agent, an initiator, a nucleating agent, glass fiber (unmodified glass fiber), GMA, modified glass fiber and a compound antioxidant;
the glass fiber reinforced polyamide composite materials of comparative examples 1 to 5 were prepared in the same manner as in examples 1 to 6.
The specific amounts (parts by weight) of the components are shown in table 2.
TABLE 2
The rest is the same as in examples 1 to 6.
And (3) performance detection:
the polyamide composite materials of examples 1 to 6 and comparative examples 1 to 5 were tested, and the specific test data are shown in tables 3 and 4.
TABLE 3
TABLE 4
The relevant performance tests were referenced to the following criteria, specific gravity: ASTM D792; notched impact strength: ASTM D256, kJ/m2(ii) a Tensile strength: ASTM D638, MPa; elongation at breakRate: ASTM D638 (%); bending strength: ASTM D790, MPa; flexural modulus: ASTM D790, MPa; heat distortion temperature: ASTM D648, 0.45MPa, unannealed, ° C; equilibrium water absorption and saturated water absorption: ASTM D570 (%).
And (4) conclusion: referring to tables 3 and 4, it can be seen from examples 1 to 6 and comparative examples 1 to 5 that the glass fiber coated and modified by GMA is more favorable for improving the mechanical properties of the polyamide composite material and the property retention rate after high-temperature water boiling compared with the common glass fiber, and simultaneously, the addition of GMA can effectively avoid the degradation of the polyamide molecular chain, reduce the molecular weight, improve the melt index and ensure the melt strength and the mechanical properties. It can be seen from example 3 and comparative examples 1 and 5 that GMA is separately mixed with resin and added into the formula without being coated with glass fiber in advance, although the enhancement effect on the polyamide composite material is achieved, the enhancement effect is not as fine as that achieved by coating GMA with glass fiber, and meanwhile, due to the addition of the initiator, the epoxy group of GMA can be effectively opened, the chain extension effect on the polyamide molecular chain is achieved, the molecular weight is not reduced, and the mechanical property of the material is improved.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. The hydrolysis-resistant glass fiber reinforced polyamide composite material is characterized by being prepared from the following components in parts by weight: 30-80 parts of polyamide resin, 0.5-1.0 part of dispersing agent, 3-10 parts of toughening agent, 0.05-0.2 part of initiator, 0.1-0.2 part of nucleating agent, 10-50 parts of modified glass fiber and 0.2-0.4 part of antioxidant; wherein the modified glass fiber is glass fiber with the outer surface coated with glycidyl methacrylate.
2. The hydrolysis-resistant glass fiber reinforced polyamide composite material of claim 1, wherein the glass fiber is an alkali-free continuous glass fiber having a diameter of 10 to 17 microns.
3. The hydrolysis-resistant glass fiber reinforced polyamide composite material as claimed in claim 1, wherein the preparation method of the modified glass fiber comprises the following steps:
a device preparation step: providing modification equipment, wherein the modification equipment comprises a pipeline, and a spraying device and a drying device are sequentially arranged in the pipeline along the glass fiber conveying direction;
spraying: sending the glass fiber into a pipeline, and spraying GMA on the outer surface of the glass fiber through a spraying device when the glass fiber moves to the position of the spraying device, so that the GMA uniformly coats the surface of the glass fiber;
and (3) drying: and after the spraying step is finished, continuously conveying the glass fibers, and drying the glass fibers by using a drying device when the glass fibers move to the position of the drying device to obtain the modified glass fibers.
4. The hydrolysis-resistant glass fiber reinforced polyamide composite material as claimed in claim 3, wherein in the drying step, the drying temperature is 130-150 ℃ and the drying distance is 0.5-1.0 m.
5. The hydrolysis-resistant glass fiber reinforced polyamide composite material as claimed in claim 1, wherein the antioxidant is one or more of antioxidant 168, antioxidant 626, antioxidant 1098, antioxidant 1010 and antioxidant 1076.
6. The hydrolysis-resistant glass fiber reinforced polyamide composite material as claimed in claim 1, wherein the polyamide resin is a polyamide resin having a relative viscosity of 2.5 to 3.0.
7. The hydrolysis-resistant glass fiber reinforced polyamide composite material of claim 1, wherein the dispersant is a hyperbranched resin, and the toughening agent is one or more of POE-g-MAH, SEBS-g-MAH, EMA and EBA; the initiator is di-tert-butyl peroxide, and the nucleating agent is long-carbon-chain carboxylate.
8. A method for preparing the hydrolysis-resistant glass fiber reinforced polyamide composite material according to any one of claims 1 to 7, which is characterized by comprising the following steps:
mixing: drying polyamide resin, mixing the dried polyamide resin, a dispersing agent, a toughening agent, an initiator, nucleation and an antioxidant in a high-speed mixer according to a formula ratio, and fully stirring and uniformly dispersing to obtain a mixed material;
an extrusion step: adding the mixed material into a double-screw extruder from a feed inlet of the double-screw extruder, adding the modified glass fiber with the formula amount into the double-screw extruder from an exhaust port of the double-screw extruder, and performing melt extrusion to obtain an extruded material;
and (3) pelletizing: and (4) bracing, cooling, air-drying, granulating and mixing the extruded materials.
9. The method for preparing the hydrolysis-resistant glass fiber reinforced polyamide composite material as claimed in claim 8, wherein the method further comprises the steps of strong magnetism treatment, mixing and homogenization treatment after the step of granulating.
10. The method for preparing the hydrolysis-resistant glass fiber reinforced polyamide composite material as claimed in claim 8, wherein in the mixing step, the drying temperature of the polyamide resin is 110 ℃, the drying time is 4h, the mixing temperature is normal temperature, and the mixing speed is 200-300 r/min; in the extrusion step, the length-diameter ratio of the twin-screw extruder is 48/1; the melt extrusion temperature is 200-260 ℃, and the screw rotating speed is 300-500 r/m.
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| CN105694447B (en) * | 2016-03-09 | 2018-01-26 | 深圳华力兴新材料股份有限公司 | A kind of NMT Amilan polyamide resin compositions for possessing LDS functions |
| CN108456371A (en) * | 2018-02-07 | 2018-08-28 | 晖腾工业科技有限公司 | A kind of modified AS resin composite materials |
| CN111484735A (en) * | 2020-04-17 | 2020-08-04 | 广东圆融新材料有限公司 | Polyamide 6 composition and preparation method thereof |
| CN112409783B (en) * | 2020-10-27 | 2022-09-02 | 东莞市鑫塑源塑胶科技有限公司 | Hydrolysis-resistant nylon composite material for automobiles and preparation method thereof |
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| CN116655964B (en) * | 2023-06-30 | 2024-03-29 | 江苏普非尔塑料科技有限公司 | High-weather-resistance high-rigidity polyamide composite material and preparation process thereof |
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