CN114249940A - Long glass fiber reinforced polypropylene composite material and preparation method thereof - Google Patents
Long glass fiber reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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- CN114249940A CN114249940A CN202010994859.4A CN202010994859A CN114249940A CN 114249940 A CN114249940 A CN 114249940A CN 202010994859 A CN202010994859 A CN 202010994859A CN 114249940 A CN114249940 A CN 114249940A
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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
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- 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
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/14—Copolymers of propene
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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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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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
- 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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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
Abstract
The invention belongs to the field of high polymer materials, and particularly relates to a long glass fiber reinforced polypropylene composite material and a preparation method thereof, wherein the composite material comprises the following raw material components in percentage by weight: 30-80% of polypropylene, 5-60% of long glass fiber, 0.1-5.0% of hyperbranched polyethylene, 1-10% of compatilizer, 0.2-2.0% of heat stabilizer and 0.2-2.0% of light stabilizer. A preparation method of a long glass fiber reinforced polypropylene composite material comprises the steps of mixing polypropylene, a compatilizer, hyperbranched polyethylene, a heat stabilizer and a light stabilizer, adding the mixture into a double-screw extruder, connecting an impregnation die of long glass fibers to the head of the double-screw extruder, fusing the long glass fibers with a polypropylene melt through the impregnation die, and carrying out melt blending, water cooling and particle cutting through the double-screw extruder to obtain the polypropylene composite material, wherein the glass fibers are used for measuring the weight of the glass fibers through the rotating speed of a traction device, the traction speed of the long glass fibers is 10-100 m/min, and the temperature of the long glass fibers through the impregnation die is 200-300 ℃. Compared with the prior art, the toughness index is improved.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to a long glass fiber reinforced polypropylene composite material and a preparation method thereof.
Background
The polypropylene is an imported plastic raw material with large dosage, and the polypropylene is reinforced by long glass fibers, so that the polypropylene has ultrahigh strength and good processability. The invention patent with the prior patent application number of CN200810020936.5 discloses a long glass fiber reinforced polypropylene material and a preparation method thereof, and the composite material comprises the following components in percentage by mass: 35-55 wt% of polypropylene, 35-50 wt% of long glass fiber, 0.3-0.8 wt% of coupling agent, 5-10 wt% of compatilizer, 2-4 wt% of flow modifier, 0.3-0.6 wt% of antioxidant and 1-2 wt% of lubricant, wherein the flow modifier is PP cooling master batch. The polypropylene material still has the defects of unstable melt mass flow rate, overlarge product smell caused by PP cooling master batches and the like.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a long glass fiber reinforced polypropylene composite material and a preparation method thereof.
The specific technical scheme of the invention is as follows:
a long glass fiber reinforced polypropylene composite material comprises the following raw material components in percentage by weight: 30-80% of polypropylene, 5-60% of long glass fiber, 0.1-5.0% of hyperbranched polyethylene, 1-10% of compatilizer, 0.2-2.0% of heat stabilizer and 0.2-2.0% of light stabilizer.
Wherein, preferably, the raw material components and weight percentage are as follows: 30% of polypropylene, 60% of long glass fiber, 2% of hyperbranched polyethylene, 6% of compatilizer, 1% of heat stabilizer and 1% of light stabilizer.
Preferably, the polypropylene is homo-polypropylene, co-polypropylene or a mixture of the homo-polypropylene and the co-polypropylene, and the melt flow rate of the polypropylene is 10-200 g/10 min; the long glass fiber is alkali-free continuous long glass fiber, and the diameter of the glass fiber is 5-25 mu m; the light stabilizer is one or more of hindered amine light stabilizers; the compatilizer is at least one of silane coupling agent and maleic anhydride graft (PP-g-MAH); the heat stabilizer is one or more of aromatic amine antioxidant, hindered phenol antioxidant, phosphite antioxidant and thiodipropionic acid diester.
Wherein, preferably, when the compatilizer is maleic anhydride graft, the polymer matrix is selected from one or more of polyethylene, polypropylene, ethylene-alpha-ethylene-octene copolymer, and copolymer of styrene and butadiene, and the polar monomer is selected from one or more of maleic anhydride and analogues thereof, or acrylic acid and ester derivatives thereof.
Wherein, preferably, the polar monomer, maleic anhydride and the like is fumaric acid; the acrylic acid and the ester derivatives thereof are one or more of acrylic acid, methacrylic acid, methyl acrylate and ethyl acrylate.
Wherein, preferably, the hindered phenol antioxidant is an antioxidant 1010, and the phosphite antioxidant is an antioxidant 168; the hindered amine light stabilizer is 994 or 770.
Preferably, the weight average molecular weight of the hyperbranched polyethylene is 20-80 ten thousand, and the branching rate is 8-80/1000C.
A preparation method of a long glass fiber reinforced polypropylene composite material comprises the steps of mixing polypropylene, a compatilizer, hyperbranched polyethylene, a heat stabilizer and a light stabilizer, adding the mixture into a double-screw extruder, connecting an impregnation die of long glass fibers to the head of the double-screw extruder, fusing the long glass fibers with a polypropylene melt through the impregnation die, and carrying out melt blending, water cooling and particle cutting through the double-screw extruder to obtain the polypropylene composite material, wherein the glass fibers are used for measuring the weight of the glass fibers through the rotating speed of a traction device, the traction speed of the long glass fibers is 10-100 m/min, and the temperature of the long glass fibers through the impregnation die is 200-300 ℃.
Advantageous effects
The hyperbranched polyethylene is added in the polypropylene, compatilizer, long glass fiber, heat stabilizer and light stabilizer system, compared with the system without the hyperbranched polyethylene, the toughness index of the long glass fiber reinforced polypropylene is improved, the rigidity change is not large, the rigidity balance is more excellent, the long glass fiber reinforced polypropylene prepared by the process is suitable for injection molding of molded automobile interior and exterior parts with certain toughness requirements, and the molding requirements of large-scale parts can be met.
Detailed Description
In the following examples, the polypropylene is a commercially available grade, the long glass fiber is an alkali-free long glass fiber, the hyperbranched polyethylene is synthesized in a laboratory according to the existing method, and the compatibilizer, the heat stabilizer and the light stabilizer are all commercially available.
In the following examples, the prepared long glass fiber reinforced polypropylene was tested for Izod impact strength according to GB/T1843-2008, bending property according to GB/T9341-2008, and tensile property according to GB/T1040.1-2018.
Example 1
The composition of the long glass fiber reinforced polypropylene described in this example is shown in Table 1.
The preparation method of the long glass fiber reinforced polypropylene comprises the following steps:
(1) firstly, mixing polypropylene, a compatilizer, hyperbranched polyethylene, a heat stabilizer and a light stabilizer, and adding the mixture into a double-screw extruder, wherein the stirring speed of the double-screw extruder is 300 revolutions per minute, and the temperature is 180-260 ℃;
(2) the long glass fiber is fused with the polypropylene melt through an impregnation die, and the long glass fiber is drawn into the long glass fiber through the impregnation die at the speed of 80 m/min. And finally obtaining the long glass fiber reinforced polypropylene through melt blending, water cooling and grain cutting by a double-screw extruder. The length-diameter ratio L/D of the double-screw extruder is 45, and after feeding through a feeding port, the materials are melted, mixed and extruded for granulation. The process comprises the following steps: the temperature of the first area is 170-190 ℃, the temperature of the second area is 190-210 ℃, the temperature of the third area is 210-230 ℃, and the temperature of the fourth area is 230-250 ℃; the temperature of the dipping die is 240-260 ℃, the residence time of the whole extrusion process is about 1 minute, and the pressure is 18 MPa.
The prepared long glass fiber reinforced polypropylene is made into national standard sample bars, and the performance measured in a standard laboratory is shown in table 2.
Example 2
The composition of the long glass fiber reinforced polypropylene described in this example is shown in Table 1.
The preparation method of the long glass fiber reinforced polypropylene comprises the following steps:
(1) firstly, mixing polypropylene, a compatilizer, hyperbranched polyethylene, a heat stabilizer and a light stabilizer, adding the mixture into a double-screw extruder, wherein the stirring speed of the double-screw extruder is 300 revolutions per minute, and the temperature is 180-260 ℃;
(2) the long glass fiber is fused with the polypropylene melt through an impregnation die, and the long glass fiber is drawn into the long glass fiber through the impregnation die at a speed of 100 m/min. And finally obtaining the long glass fiber reinforced polypropylene through melt blending, water cooling and grain cutting by a double-screw extruder. The length-diameter ratio L/D of the double-screw extruder is 45, and after feeding through a feeding port, the materials are melted, mixed and extruded for granulation. The process comprises the following steps: the temperature of the first area is 170-190 ℃, the temperature of the second area is 190-210 ℃, the temperature of the third area is 210-230 ℃, and the temperature of the fourth area is 230-250 ℃; the temperature of the dipping die is 280-300 ℃, the residence time of the whole extrusion process is about 1 minute, and the pressure is 18 MPa.
The prepared long glass fiber reinforced polypropylene is made into national standard sample bars, and the performance measured in a standard laboratory is shown in table 2.
Example 3
The composition of the long glass fiber reinforced polypropylene described in this example is shown in Table 1.
The preparation method of the long glass fiber reinforced polypropylene comprises the following steps:
(1) firstly, mixing polypropylene, a compatilizer, hyperbranched polyethylene, a heat stabilizer and a light stabilizer, adding the mixture into a double-screw extruder, wherein the stirring speed of the double-screw extruder is 300 revolutions per minute, and the temperature is 180-260 ℃;
(2) the long glass fiber is fused with the polypropylene melt through an impregnation die, and the long glass fiber is drawn into the long glass fiber through the impregnation die at a speed of 50 m/min. And finally obtaining the long glass fiber reinforced polypropylene through melt blending, water cooling and grain cutting by a double-screw extruder. The length-diameter ratio L/D of the double-screw extruder is 45, and after feeding through a feeding port, the materials are melted, mixed and extruded for granulation. The process comprises the following steps: the temperature of the first area is 170-190 ℃, the temperature of the second area is 190-210 ℃, the temperature of the third area is 210-230 ℃, and the temperature of the fourth area is 230-250 ℃; the temperature of the dipping die is 200-220 ℃, the residence time of the whole extrusion process is about 1 minute, and the pressure is 18 MPa.
The prepared long glass fiber reinforced polypropylene is made into national standard sample bars, and the performance measured in a standard laboratory is shown in table 2.
Example 4
The composition of the long glass fiber reinforced polypropylene described in this example is shown in Table 1.
The preparation method of the long glass fiber reinforced polypropylene comprises the following steps:
(1) firstly, mixing polypropylene, a compatilizer, hyperbranched polyethylene, a heat stabilizer and a light stabilizer, adding the mixture into a double-screw extruder, wherein the stirring speed of the double-screw extruder is 300 revolutions per minute, and the temperature is 180-260 ℃;
(2) the long glass fiber is fused with the polypropylene melt through an impregnation die, and the long glass fiber is drawn into the long glass fiber through the impregnation die at the speed of 30 m/min. And finally obtaining the long glass fiber reinforced polypropylene through melt blending, water cooling and grain cutting by a double-screw extruder. The length-diameter ratio L/D of the double-screw extruder is 45, and after feeding through a feeding port, the materials are melted, mixed and extruded for granulation. The process comprises the following steps: the temperature of the first area is 170-190 ℃, the temperature of the second area is 190-210 ℃, the temperature of the third area is 210-230 ℃, and the temperature of the fourth area is 230-250 ℃; the temperature of the dipping die is 260-280 ℃, the residence time of the whole extrusion process is about 1 minute, and the pressure is 18 MPa.
The prepared long glass fiber reinforced polypropylene is made into national standard sample bars, and the performance measured in a standard laboratory is shown in table 2.
Example 5
The composition of the long glass fiber reinforced polypropylene described in this example is shown in Table 1.
The preparation method of the long glass fiber reinforced polypropylene comprises the following steps:
(1) firstly, mixing polypropylene, a compatilizer, hyperbranched polyethylene, a heat stabilizer and a light stabilizer, adding the mixture into a double-screw extruder, wherein the stirring speed of the double-screw extruder is 300 revolutions per minute, and the temperature is 180-260 ℃;
(2) the long glass fiber is fused with the polypropylene melt through an impregnation die, and the long glass fiber is drawn into the long glass fiber through the impregnation die at a speed of 10 m/min. And finally obtaining the long glass fiber reinforced polypropylene through melt blending, water cooling and grain cutting by a double-screw extruder. The length-diameter ratio L/D of the double-screw extruder is 45, and after feeding through a feeding port, the materials are melted, mixed and extruded for granulation. The process comprises the following steps: the temperature of the first area is 170-190 ℃, the temperature of the second area is 190-210 ℃, the temperature of the third area is 210-230 ℃, and the temperature of the fourth area is 230-250 ℃; the temperature of the dipping die is 220-240 ℃, the residence time of the whole extrusion process is about 1 minute, and the pressure is 18 MPa.
The prepared long glass fiber reinforced polypropylene is made into national standard sample bars, and the performance measured in a standard laboratory is shown in table 2.
Comparative example 1
The composition of the long glass fiber reinforced polypropylene of this comparative example is shown in Table 1.
The preparation method of the long glass fiber reinforced polypropylene of the comparative example comprises the following steps:
(1) firstly, mixing polypropylene, a compatilizer, a heat stabilizer and a light stabilizer, adding the mixture into a double-screw extruder, wherein the stirring speed of the double-screw extruder is 300 revolutions per minute, and the temperature is 180-260 ℃;
(2) the long glass fiber is fused with the polypropylene melt through an impregnation die, and the long glass fiber is drawn into the long glass fiber through the impregnation die at a speed of 50 m/min. And finally obtaining the long glass fiber reinforced polypropylene through melt blending, water cooling and grain cutting by a double-screw extruder.
The prepared long glass fiber reinforced polypropylene is made into national standard sample bars, and the performance measured in a standard laboratory is shown in table 2.
TABLE 1 formulation tables for examples 1-5 and comparative example 1
TABLE 2 spline test results for examples 1-5 and comparative example 1
It can be seen from the comparison between examples 1-5 and comparative example 1 that the hyperbranched polyethylene and the polypropylene system are blended, so that the toughness of the material can be improved, compared with the method without adding the hyperbranched polyethylene, the normal-temperature cantilever beam impact strength is improved to different degrees, the rigidity change indicated by the flexural modulus and the flexural strength is not large, the rigidity and toughness balance is more excellent, and the long glass fiber reinforced polypropylene prepared by the process is suitable for injection molding of molded automobile interior and exterior parts with certain toughness requirements, and can meet the molding requirements of large-scale parts.
Claims (8)
1. The long glass fiber reinforced polypropylene composite material is characterized by comprising the following raw material components in percentage by weight: 30-80% of polypropylene, 5-60% of long glass fiber, 0.1-5.0% of hyperbranched polyethylene, 1-10% of compatilizer, 0.2-2.0% of heat stabilizer and 0.2-2.0% of light stabilizer.
2. The polypropylene composite material according to claim 1, wherein the polypropylene composite material comprises the following raw material components in percentage by weight: 30% of polypropylene, 60% of long glass fiber, 2% of hyperbranched polyethylene, 6% of compatilizer, 1% of heat stabilizer and 1% of light stabilizer.
3. The long glass fiber reinforced polypropylene according to claim 1 or 2, wherein:
the polypropylene is homo-polypropylene, co-polypropylene or a mixture of the homo-polypropylene and the co-polypropylene, and the melt flow rate of the polypropylene is 10-200 g/10 min;
the long glass fiber is alkali-free continuous long glass fiber, and the diameter of the glass fiber is 5-25 mu m;
the light stabilizer is one or more of hindered amine light stabilizers;
the compatilizer is at least one of silane coupling agent and polar monomer graft polymer;
the heat stabilizer is one or more of aromatic amine antioxidant, hindered phenol antioxidant, phosphite antioxidant and thiodipropionic acid diester.
4. The polypropylene composite of claim 3, wherein when the compatibilizer is a polar monomer graft polymer, the polymer matrix is selected from one or more of polyethylene, polypropylene, ethylene- α -ethylene-octene copolymer, and a copolymer of styrene and butadiene, and the polar monomer is selected from one or more of maleic anhydride and its analogs, or acrylic acid and its ester derivatives.
5. The polypropylene composite according to claim 4, wherein in the polar monomer, the analogue of maleic anhydride is fumaric acid; the acrylic acid and the ester derivatives thereof are one or more of acrylic acid, methacrylic acid, methyl acrylate and ethyl acrylate.
6. The polypropylene composite of claim 3, wherein the hindered phenolic antioxidant is antioxidant 1010 and the phosphite antioxidant is antioxidant 168; the hindered amine light stabilizer is 994 or 770.
7. The polypropylene composite material according to claim 1, wherein the hyperbranched polyethylene has a weight average molecular weight of 20 to 80 ten thousand and a branching ratio of 8 to 80/1000C.
8. A preparation method of a long glass fiber reinforced polypropylene composite material is characterized in that polypropylene, a compatilizer, hyperbranched polyethylene, a heat stabilizer and a light stabilizer are mixed and added into a double-screw extruder, an impregnation die of long glass fiber is connected to the head of the double-screw extruder, the long glass fiber is fused with polypropylene melt through the impregnation die, and the polypropylene composite material can be obtained through melt blending, water cooling and grain cutting of the double-screw extruder,
wherein the weight of the glass fiber is measured by the rotating speed of the traction device, the traction speed of the long glass fiber is 10-100 m/min, and the temperature of the long glass fiber passing through the dipping die is 200-300 ℃.
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