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CN110423461B - Low-water-absorption flame-retardant glass fiber reinforced PA6 composite material and preparation method thereof - Google Patents

Low-water-absorption flame-retardant glass fiber reinforced PA6 composite material and preparation method thereof Download PDF

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CN110423461B
CN110423461B CN201910709922.2A CN201910709922A CN110423461B CN 110423461 B CN110423461 B CN 110423461B CN 201910709922 A CN201910709922 A CN 201910709922A CN 110423461 B CN110423461 B CN 110423461B
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temperature
antioxidant
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processing aid
glass fiber
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陆龙威
鲁淞彥
胡鑫斌
郝刘佳
王晓东
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Hengdian Group Debang Engineering Plastic Co ltd
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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
    • 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
    • C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • 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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    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477—Six-membered rings
    • C08K5/3492—Triazines
    • C08K5/34922—Melamine; Derivatives thereof
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    • 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
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Abstract

The invention belongs to the field of high polymer materials, and discloses a low-water-absorption flame-retardant glass fiber reinforced PA6 composite material and a preparation method thereof. The low-water-absorption flame-retardant glass fiber reinforced PA6 composite material comprises, by weight, 43.6-99.3 parts of PA6, 5.0-15.0 parts of a hydrophobizing agent, 10.0-30.0 parts of glass fibers, 5.0-20.0 parts of a flame retardant, 0.2-0.4 part of an antioxidant and 0.5-1 part of a processing aid. According to the invention, the molding process of the low-water-absorption flame-retardant toughened PA6 composite material is optimized, the hydrophobic performance of a PA6 matrix is improved by using stearic acid and ammonium stearate, the flame retardant performance of the material is improved by MPP, and the mechanical properties such as impact strength, tensile strength, elongation at break and the like of the PA6 are improved by adding glass fibers, wherein the stearic acid and the ammonium stearate can increase the compatibility of MPP and the PA6 matrix and inhibit the precipitation, in addition, the hydrophobing agent is heated and decomposed to generate gas and simultaneously has a gas-phase flame-retardant effect, a melamine group in the MPP structure has a certain hydrophobic performance, and the two materials simultaneously have the effects of synergistic flame retardance and synergistic hydrophobicity.

Description

Low-water-absorption flame-retardant glass fiber reinforced PA6 composite material and preparation method thereof
Technical Field
The invention relates to the field of high polymer materials, in particular to a low-water-absorption flame-retardant glass fiber reinforced PA6 composite material and a preparation method thereof.
Background
Nylon 6(PA6 or polyamide 6) is an important engineering plastic widely applied to five engineering plastics, and has excellent impact resistance, higher tensile strength, good wear resistance, and excellent electrical insulation performance and chemical resistance. The material is mainly applied to the fields of hardware machinery, electronics, electrics, instruments and meters and the like. However, polyamide is easy to form intermolecular hydrogen bonds with water molecules due to amido bonds in the structure of the polyamide, so that the material is easy to absorb water, the rigidity is poor, the long-term service performance of the material is greatly influenced by the size change of the material caused by water absorption, and the use of PA6 in the field of fine elements is limited. With the continuous development of products and the gradual implementation of new standards, the industry puts higher demands on the tensile strength and toughness of nylon 6. In addition, PA6 belongs to combustible materials, generates molten drops and dense smoke after combustion, accelerates the diffusion and spread of flame, and needs flame retardant modification before use. Therefore, low water absorption enhanced PA6 is a major direction in the research of such materials at present.
Disclosure of Invention
The invention aims to overcome the defects of the background technology and provides a low-water-absorption flame-retardant glass fiber reinforced PA6 composite material and a preparation method thereof. The flame-retardant glass fiber reinforced PA6 composite material with low water absorption is prepared by modifying PA6 with stearic acid and ammonium stearate to improve the hydrophobicity, and MPP is used as a flame retardant and has the synergistic functions of compatibility and flame retardance with the stearic acid and the ammonium stearate. Compared with the traditional PA6, the product has low water absorption and excellent flame retardant property. Meanwhile, the glass fiber is low in addition amount, the whole additive is low in proportion, the cost is reduced, and the cost performance is higher.
In order to achieve the purpose of the invention, the low-water-absorption flame-retardant glass fiber reinforced PA6 composite material comprises, by weight, 43.6-99.3 parts of PA6, 5.0-15.0 parts of a hydrophobizing agent, 10.0-30.0 parts of glass fiber, 5.0-20.0 parts of a flame retardant, 0.2-0.4 part of an antioxidant and 0.5-1 part of a processing aid.
Further, the hydrophobic agent is one or more of stearic acid and ammonium stearate.
Further, the flame retardant is one or more of melamine polyphosphate (MPP), Melamine Cyanurate (MCA) and melamine.
Further, the antioxidant is one or more of antioxidant 1010, antioxidant 168, antioxidant 1076, antioxidant 264 and antioxidant 245.
Further, the processing aid is a mixture of a lubricant, a dispersant and an aminosilane coupling agent.
Preferably, the lubricant is one or more of stearamide, paraffin wax, polyethylene wax or polypropylene wax; the dispersing agent is a fatty acid derivative; the aminosilane coupling agent is KH-550.
In another aspect, the invention provides a preparation method of the low-water-absorption flame-retardant glass fiber reinforced PA6 composite material, and the preparation method includes:
(1) stirring the PA6 particles, the hydrophobing agent, the flame retardant, the antioxidant and the processing aid in a high-speed stirrer for 15-30 min at a stirring speed of 2500 r/min;
(2) putting the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) into a vacuum drying oven for drying;
(3) adding the mixture of the hydrophobing agent, the flame retardant, the antioxidant and the processing aid dried in the step (2) from a main feeding port, adding the glass fiber from a side feeding port, extruding in a double-screw extruder, and granulating;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form PA6 sample bars.
Preferably, the mixture in the step (2) is dried for 20-28 hours in a vacuum drying oven at the temperature of 85-95 ℃.
Preferably, in the step (3), the twin-screw parameters include that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the twin-screw is 80r/min, the rotating speed of a feeder is 6r/min, and the rotating speed of a granulator is 300 r/min.
Preferably, the temperature of each section of the single-screw injection molding machine in the step (4) is respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, and the mold temperature is 85-95 ℃.
According to the invention, the molding process of the low-water-absorption flame-retardant toughened PA6 composite material is optimized, the hydrophobic performance of a PA6 matrix is improved by using stearic acid and ammonium stearate, the flame retardant performance of the material is improved by MPP, and the mechanical properties such as impact strength, tensile strength, elongation at break and the like of PA6 are improved by adding glass fiber.
According to the invention, the stearic acid and the ammonium stearate can increase the compatibility of MPP and a PA6 matrix and inhibit precipitation, in addition, the hydrophobic agent is heated and decomposed to generate gas and simultaneously has a gas phase flame retardant effect, the melamine group in the MPP structure has a certain hydrophobic property, and the MPP structure simultaneously have the synergistic flame retardant and synergistic hydrophobic effects.
The method adopted by the invention has the advantages of simple processing and forming, low cost of formula components, no heavy metal and halogen elements, environmental protection and low energy consumption.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
According to the invention, stearic acid and ammonium stearate as hydrophobing agents simultaneously have a hydrophilic end and a lipophilic end, the hydrophilic cation end can be effectively combined with an amido bond in PA to prevent water absorption, and the lipophilic end stearic acid group can be effectively hydrophobic to reduce the water absorption of the material. In addition, the stearic acid and the ammonium stearate have low cost and mature industrial production.
The halogen-free flame retardant melamine polyphosphate (MPP) has good flame retardant performance, but has poor compatibility with PA 6. The modification effect of stearic acid and ammonium stearate serving as hydrophobic agents on the surface of MPP can increase the compatibility of MPP and a PA6 matrix and inhibit MPP from being separated out; meanwhile, the interface bonding force of the flame retardant and the flame retardant is improved, and the influence of the flame retardant on the mechanical property of the material is reduced. In addition, ammonia gas generated by thermal decomposition of ammonium stearate has a gas-phase flame retardant effect and is flame retardant in cooperation with MPP, and a melamine group in the MPP structure has certain hydrophobic property and can be hydrophobic in cooperation with a hydrophobic agent, so that the water absorption rate is further reduced.
The glass fiber (glass fiber) has the advantages of high yield, low price and the like, is commonly used for reinforcing PA6 in industry, and can remarkably improve the mechanical properties such as impact property, elastic modulus, fatigue resistance, creep resistance and rigidity of PA6, and is also beneficial to stabilizing the size of a product and reducing the molding shrinkage rate.
The technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1
(1) Stirring 79.3 wt% of PA6 particles, 5wt% of stearic acid, 5wt% of MPP, 0.2wt% of antioxidant (0.1 wt% of antioxidant 168 and 0.1 wt% of antioxidant 1010 respectively) and 0.5 wt% of processing aid (0.1 wt% of fatty glyceride, 0.1 wt% of paraffin and 0.3 wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 10 wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min, and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Example 2
(1) Stirring 79.3 wt% of PA6 particles, 5wt% of ammonium stearate, 5wt% of MPP, 0.2wt% of antioxidant (0.1 wt% of antioxidant 168 and antioxidant 1010 respectively) and 0.5 wt% of processing aid (0.1 wt% of fatty glyceride, 0.1 wt% of paraffin and 0.3 wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 10 wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min, and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Example 3
(1) Stirring 64.3 wt% of PA6 particles, 10 wt% of stearic acid, 10 wt% of MPP, 0.2wt% of antioxidant (0.1 wt% of antioxidant 168 and 0.1 wt% of antioxidant 1010 respectively) and 0.5 wt% of processing aid (0.1 wt% of fatty glyceride, 0.1 wt% of paraffin and 0.3 wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 15wt% of the mixture from a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of double screws are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screws is 80r/min, the rotating speed of a feeding machine is 6r/min and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Example 4
(1) Stirring 64.3 wt% of PA6 particles, 10 wt% of ammonium stearate, 10 wt% of MPP, 0.2wt% of antioxidant (0.1 wt% of antioxidant 168 and antioxidant 1010 respectively) and 0.5 wt% of processing aid (0.1 wt% of fatty glyceride, 0.1 wt% of paraffin and 0.3 wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 15wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Example 5
(1) Stirring 48.6wt% of PA6 particles, 15wt% of stearic acid, 15wt% of MPP, 0.4wt% of antioxidant (0.2 wt% of antioxidant 168 and antioxidant 1010 respectively) and 1wt% of processing aid (0.2 wt% of fatty glyceride, 0.2wt% of paraffin and 0.6wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 20wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Example 6
(1) Stirring 48.6wt% of PA6 particles, 15wt% of ammonium stearate, 15wt% of MPP, 0.4wt% of antioxidant (0.2 wt% of antioxidant 168 and antioxidant 1010 respectively) and 1wt% of processing aid (0.2 wt% of fatty glyceride, 0.2wt% of paraffin and 0.6wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 20wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Example 7
(1) Stirring 48.6wt% of PA6 particles, 15wt% of ammonium stearate, 20wt% of MCA, 0.4wt% of antioxidant (0.2 wt% of antioxidant 168 and antioxidant 1010 respectively) and 1wt% of processing aid (0.2 wt% of fatty glyceride, 0.2wt% of paraffin and 0.6wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 15wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Example 8
(1) Stirring 48.6wt% of PA6 particles, 15wt% of ammonium stearate, 15wt% of melamine, 0.4wt% of antioxidant (0.2 wt% of antioxidant 168 and 0.2wt% of antioxidant 1010 respectively) and 1wt% of processing aid (0.2 wt% of fatty glyceride, 0.2wt% of paraffin and 0.6wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 20wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Example 9
(1) Stirring 48.6wt% of PA6 particles, 10 wt% of ammonium stearate, 15wt% of MPP, 0.4wt% of antioxidant (0.2 wt% of antioxidant 168 and antioxidant 1010 respectively) and 1wt% of processing aid (0.2 wt% of fatty glyceride, 0.2wt% of paraffin and 0.6wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 25 wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Example 10
(1) Stirring 43.6 wt% of PA6 particles, 10 wt% of ammonium stearate, 15wt% of MPP, 0.4wt% of antioxidant (0.2 wt% of antioxidant 168 and antioxidant 1010 respectively) and 1wt% of processing aid (0.2 wt% of fatty glyceride, 0.2wt% of paraffin and 0.6wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 30 wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min, and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Comparative example 1
(1) Stirring 99.3 wt% of PA6 particles, 0.2wt% of antioxidant (0.1 wt% of antioxidant 168 and antioxidant 1010 respectively) and 0.5 wt% of processing aid (0.1 wt% of fatty glyceride, 0.1 wt% of paraffin and 0.3 wt% of KH-550) in a high-speed stirrer for 10min at the stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles, the antioxidant and the processing aid dried in the step (2) from a main feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of the double screws are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screws is 80r/min, the rotating speed of the feeder is 6r/min, and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Comparative example 2
(1) Stirring 84.3 wt% of PA6 particles, 15wt% of ammonium stearate, 0.2wt% of antioxidant (0.1 wt% of antioxidant 168 and antioxidant 1010 respectively) and 0.5 wt% of processing aid (0.1 wt% of fatty glyceride, 0.1 wt% of paraffin and 0.3 wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), the hydrophobing agent, the antioxidant and the processing aid from a main feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of the double screws are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screws is 80r/min, the rotating speed of the feeder is 6r/min, and the rotating speed of the granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s. Comparative example 3
(1) Stirring 79.3 wt% of PA6 particles, 20wt% of MPP, 0.2wt% of antioxidant (0.1 wt% of antioxidant 168 and antioxidant 1010 respectively) and 0.5 wt% of processing aid (0.1 wt% of fatty glyceride, 0.1 wt% of paraffin and 0.3 wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), the flame retardant, the antioxidant and the processing aid from a main feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of the double screws are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screws is 80r/min, the rotating speed of the feeder is 6r/min, and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
Comparative example 4
(1) Stirring 69.3 wt% of PA6 particles, 0.2wt% of antioxidant (0.1 wt% of antioxidant 168 and antioxidant 1010 respectively) and 0.5 wt% of processing aid (0.1 wt% of fatty glyceride, 0.1 wt% of paraffin and 0.3 wt% of KH-550) in a high-speed stirrer for 10min at a stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles, the antioxidant and the processing aid dried in the step (2) from a main feeding port, adding 30 wt% of glass fiber at a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of double screws are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screws is 80r/min, the rotating speed of a feeder is 6r/min, and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
The composition of the materials and the results of the performance test of each example and comparative example are shown in tables 1 and 2, respectively.
TABLE 1 compositions of materials of examples and comparative examples
Figure BDA0002153374600000131
Figure BDA0002153374600000141
Figure BDA0002153374600000151
TABLE 2 Performance of the final product of each example and comparative example PA6
Figure BDA0002153374600000152
It will be understood by those skilled in the art that the foregoing is merely exemplary of the present invention, and is not intended to limit the invention to the particular forms disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.

Claims (2)

1. The low-water-absorption flame-retardant glass fiber reinforced PA6 composite material is characterized in that the low-water-absorption flame-retardant glass fiber reinforced PA6 composite material comprises 48.6wt% of PA6, 15wt% of a hydrophobic agent, 20wt% of glass fiber, 15wt% of a flame retardant, 0.4wt% of an antioxidant and 1wt% of a processing aid in percentage by weight;
the hydrophobic agent is ammonium stearate;
the flame retardant is MPP;
the antioxidant consists of 0.2wt% of antioxidant 168 and antioxidant 1010 respectively;
the processing aid consists of 0.2wt% of fatty glyceride, 0.2wt% of paraffin and 0.6wt% of KH-550.
2. The preparation method of the low water absorption flame retardant glass fiber reinforced PA6 composite material of claim 1, characterized in that the preparation method comprises the following steps:
(1) stirring the PA6 particles, the hydrophobing agent, the flame retardant, the antioxidant and the processing aid in a high-speed stirrer for 10min at the stirring speed of 2500 r/min;
(2) placing the mixture of the PA6 particles, the hydrophobic agent, the flame retardant, the antioxidant and the processing aid in the step (1) in a vacuum drying oven for drying for 24 hours at 90 ℃;
(3) adding the mixture of the PA6 particles dried in the step (2), a hydrophobing agent, a flame retardant, an antioxidant and a processing aid from a main feeding port, adding 20wt% of glass fiber into a side feeding port, extruding and granulating in a double-screw extruder, wherein the parameters of a double screw are that the temperature of a first zone is 220 +/-10 ℃, the temperature of a second zone is 230 +/-10 ℃, the temperature of a third zone is 250 +/-10 ℃, the temperature of a fourth zone is 250 +/-10 ℃, the temperature of a fifth zone is 230 +/-10 ℃, the temperature of a machine head is 220 +/-10 ℃, the rotating speed of the double screw is 80r/min, the rotating speed of a feeder is 6r/min and the rotating speed of a granulator is 300 r/min;
(4) and (4) carrying out injection molding on the particles obtained by granulation in the step (3) by using a single-screw injection molding machine to form a PA6 sample strip, wherein the temperatures of all sections of the injection molding machine are respectively 220 +/-10 ℃, 245 +/-10 ℃, 230 +/-10 ℃, the injection pressure is 90 +/-5 MPa, the pressure maintaining pressure is 50 +/-5 MPa, the mold temperature is 85-95 ℃, and the pressure maintaining pressure is 10 s.
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JP2009161900A (en) * 2009-01-20 2009-07-23 Daio Paper Corp Hydrolyzabable sanitary paper
CN103937229A (en) * 2013-01-17 2014-07-23 上海杰事杰新材料(集团)股份有限公司 Fire retardant glass fiber reinforced nylon composite material, and preparation method thereof
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