CN109054189B - Plant composite fiber filled polypropylene composite material and preparation method thereof - Google Patents
Plant composite fiber filled polypropylene composite material and preparation method thereof Download PDFInfo
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- CN109054189B CN109054189B CN201810935961.XA CN201810935961A CN109054189B CN 109054189 B CN109054189 B CN 109054189B CN 201810935961 A CN201810935961 A CN 201810935961A CN 109054189 B CN109054189 B CN 109054189B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention relates to a plant composite fiber filled polypropylene composite material and a preparation method thereof. The plant composite fiber filled polypropylene composite material comprises the following raw materials in percentage by weight: 42-64% of copolymerized polypropylene, 6-18% of homopolymerized polypropylene, 5-18% of plant powder, 0-5% of inorganic mineral filler, 1-5% of elastomer, 0.8-3% of compatibilizer, 0.2-0.6% of coupling agent, 0.1-0.3% of antioxidant, 10-28% of polyester resin, 0.01-0.03% of epoxy resin and 0.03-0.08% of graphene.
Description
Technical Field
The invention relates to a plant composite fiber filled polypropylene composite material and a preparation method thereof, belonging to the technical field of environmental protection and light weight of polypropylene and composite materials thereof.
Background
The crop straws with the most similar structure to the wood have improper treatment modes such as waste, combustion and the like, and have negative effects on environmental protection and resource utilization. The vegetable fiber has fatal defects such as irregular shape, more structural defects and poor compatibility with a polymer matrix, so that the composite material has poor comprehensive performance and limited application range.
At present, the mainstream plant fiber/polypropylene composite material has the defects of large defect, poor mechanical property, poor fluidity and rough surface, and can only be applied to low-end products.
The invention develops the plant fiber/polypropylene composite material which has lower density and more stable melt fluidity while ensuring excellent mechanical property and appearance, and realizes the purposes of environmental protection and light weight of the vehicle high polymer material.
Disclosure of Invention
In order to solve the above problems, the present invention provides a plant composite fiber-filled polypropylene composite material having a lower density and a more stable melt flowability while ensuring excellent mechanical properties and appearance.
The invention also aims to provide a preparation method of the plant composite fiber filled polypropylene composite material.
The technical scheme adopted by the invention is as follows:
the plant composite fiber filled polypropylene composite material is characterized by comprising the following raw materials in percentage by weight: 42-64% of copolymerized polypropylene, 6-18% of homopolymerized polypropylene, 5-18% of plant powder, 0-5% of inorganic mineral filler, 1-5% of elastomer, 0.8-3% of compatibilizer, 0.2-0.6% of coupling agent, 0.1-0.3% of antioxidant, 10-28% of polyester resin, 0.01-0.03% of epoxy resin and 0.03-0.08% of graphene.
Further, the plant powder is at least one of straw powder, bamboo powder and wood powder.
Further, the inorganic mineral filler is hollow glass beads, the average particle size is 0.8-85 micrometers, and the specific surface area is 9-17 m 2/g.
Further, the elastomer is at least one of POE, EPDM, SBS and SEBS.
Further, the compatibilizer is at least one of SEBS-g-MAH, PP-g-MAH and POE-g-MAH.
Further, the coupling agent is a silane coupling agent KH 560.
Further, the antioxidant is an antioxidant 1010.
A method for preparing the plant composite fiber filled polypropylene composite material according to claim 1, which comprises the following steps:
(1) adding plant powder and an ethanol solution containing 1-3 wt% of a coupling agent into a high-speed stirrer for mixing, gradually adding a solution containing 1% of epoxy resin and 3% of graphene, continuously stirring for 30 minutes at 85 ℃, and drying to obtain a graphene-coated plant powder filler, wherein the particle size range of the graphene-coated plant powder filler is 15-110 micrometers;
(2) carrying out melt blending on graphene-coated plant powder filler and polyester resin, dissolving the blend with a dimethylformamide solvent, spinning and drying to form composite fibers, and grinding the composite fibers in a ball mill to prepare plant composite fiber powder, wherein the length range of the plant composite fiber powder is 22-285 microns, and the length-diameter ratio is 130: 1-240: 1;
(3) when inorganic mineral fillers exist in the raw materials, mixing the inorganic mineral fillers, polypropylene and elastomer with an ethanol solution containing 1-3 wt% of a coupling agent in a high-speed mixer for 3-8 minutes at the temperature of 50-70 ℃; when the raw materials do not contain inorganic mineral fillers, mixing the polypropylene and the elastomer in a high-speed mixer for 3-8 minutes at the temperature of 50-70 ℃;
(4) and (3) placing the materials obtained in the steps (2) and (3), the compatibilizer and the antioxidant in a double-screw extruder, and performing melt extrusion and granulation.
Further, the plant powder in the step (1) comprises the following components in percentage by weight: the solution is 5: 1.
further, in the step (2), the graphene-coated plant powder filler is prepared by the following steps: polyester resin: dimethylformamide solvent is 1: 2: 12.
the invention has the beneficial effects that: the composite material has lower density and more stable melt fluidity while ensuring excellent mechanical property and appearance, and the density is lower than 0.99g/cm3. By spinning the plant fiber, the filling problem caused by the defects of irregular shape, defects and the like of the plant fiber is overcome, the strength of the polypropylene composite material is improved, and the density of the polypropylene composite material is reduced; the plant fiber powder with a certain length-diameter ratio controls the shrinkage rate of the composite material and improves the modulus; the directional arrangement of the plant fiber powder enhances the fluidity of the polypropylene composite material in a molten state; the nucleation effect of the hollow glass beads improves the strength of the composite material.
Detailed Description
The present invention will be further described with reference to the following examples, but is not limited thereto.
Example 1
The plant composite fiber filled polypropylene composite material comprises the following components:
(1) preparing 3g of silane coupling agent KH560 into 1-3 wt% of coupling agent ethanol solution; adding 100 g of straw powder and 150 g of prepared ethanol solution of a coupling agent into a high-speed stirrer for mixing, gradually adding 20 g of solution containing 1% of epoxy resin and 3% of graphene (the epoxy resin is uncured resin, the solvent is butanol, cyclohexanone or absolute ethanol can be used as well, and the like), continuously stirring for 30 minutes at 85 ℃, and drying to obtain graphene-coated plant powder filler, wherein the particle size range of the graphene-coated plant powder filler is 15-110 micrometers;
(2) carrying out melt blending on graphene-coated plant powder filler and 200 g of polyester resin, dissolving the blend with 1200 g of dimethylformamide solvent, and then spinning and drying to form composite fibers; grinding the composite fibers in a ball mill to prepare plant composite fiber powder, wherein the length range of the plant composite fiber powder is 22-285 micrometers, and the length-diameter ratio is 130: 1-240: 1;
(3) mixing 700 g of co-polypropylene, 150 g of homo-polypropylene and 30 g of POE in a high-speed mixer for 3-8 minutes at 50-70 ℃;
(4) and (3) putting the materials obtained in the steps (2) and (3), 15 g of POE-g-MAH and 2 g of antioxidant 1010 in a double-screw extruder, and performing melt extrusion and granulation.
Wherein, the length-diameter ratio of the screws of all the double-screw extruders is 48: 1, extruding and granulating in a double-screw extruder with nine zones for controlling temperature, wherein the processing temperature in one zone to nine zones is as follows in sequence: 185 ℃, 191 ℃, 187 ℃, 190 ℃, 193 ℃, 197 ℃, 192 ℃, 195 ℃, 198 ℃, 202 ℃ of the head, 28-38 HZ of the host frequency, 22-28 HZ of the feeding frequency, 2.9-3.8 MPa of the melt pressure, 0.03-0.06 MPa of the vacuum degree and 370-470 rpm of the granulator.
Example 2
The plant composite fiber filled polypropylene composite material comprises the following components:
(1) preparing 4.5g of silane coupling agent KH560 into 1-3 wt% of coupling agent ethanol solution; adding 105 g of straw powder, 30 g of bamboo powder, 15 g of wood powder and a prepared coupling agent ethanol solution into a high-speed stirrer, mixing, gradually adding 30 g of a solution containing 1% of epoxy resin and 3% of graphene (the epoxy resin is uncured resin, the solvent is butanol, cyclohexanone or absolute ethanol can be used, and the like), continuously stirring for 30 minutes at 85 ℃, and drying to obtain the graphene-coated plant powder filler, wherein the particle size range of the graphene-coated plant powder filler is 15-110 micrometers;
(2) carrying out melt blending on graphene-coated plant powder filler and 300 g of polyester resin, dissolving the blend by using 1800 g of dimethylformamide solvent, and then spinning and drying to form composite fibers; grinding the composite fibers in a ball mill to prepare plant composite fiber powder with the length range of 22-285 microns and the length-diameter ratio of 130: 1-240: 1;
(3) 1.5 g of silane coupling agent KH560 is prepared into 1-3 wt% of coupling agent ethanol solution; mixing 50 g of hollow glass beads, 630 g of polypropylene copolymer, 100 g of polypropylene homopolymer, 32 g of EPDM and the prepared coupling agent ethanol solution in a high-speed mixer for 3-8 minutes at the temperature of 50-70 ℃;
(4) and (3) putting the materials obtained in the steps (2) and (3), 30 g of PP-g-MAH and 2 g of antioxidant 1010 in a double-screw extruder, and performing melt extrusion and granulation.
Wherein, the length-diameter ratio of the screws of all the double-screw extruders is 48: 1, extruding and granulating in a double-screw extruder with nine zones for controlling temperature, wherein the processing temperature in one zone to nine zones is as follows in sequence: 185 ℃, 191 ℃, 187 ℃, 190 ℃, 193 ℃, 197 ℃, 192 ℃, 195 ℃, 198 ℃, 202 ℃ of the head, 28-38 HZ of the host frequency, 22-28 HZ of the feeding frequency, 2.9-3.8 MPa of the melt pressure, 0.03-0.06 MPa of the vacuum degree and 370-470 rpm of the granulator.
Example 3
The plant composite fiber filled polypropylene composite material comprises the following components:
(1) preparing 2.4 g of silane coupling agent KH560 into an ethanol solution containing 1-3 wt% of coupling agent; adding 64 g of straw powder, 16 g of wood powder and 120 g of prepared ethanol solution of a coupling agent into a high-speed stirrer for mixing, gradually adding 16 g of solution containing 1% of epoxy resin and 3% of graphene (the epoxy resin is uncured resin, the solvent is butanol, cyclohexanone or absolute ethanol can be used as well, and the like), continuously stirring for 30 minutes at 85 ℃, and drying to obtain the graphene-coated plant powder filler, wherein the particle size range of the graphene-coated plant powder filler is 15-110 micrometers;
(2) carrying out melt blending on graphene-coated plant powder filler and 160 g of polyester resin, dissolving the blend by using 960 g of dimethylformamide solvent, and then spinning and drying to form composite fibers; grinding the composite fibers in a ball mill to prepare plant composite fiber powder, wherein the length range of the plant composite fiber powder is 22-285 micrometers, and the length-diameter ratio is 130: 1-240: 1;
(3) preparing 0.6 g of silane coupling agent KH560 into 1-3 wt% of coupling agent ethanol solution, and mixing 20 g of hollow glass beads, 740 g of co-polypropylene, 120 g of homo-polypropylene, 22 g of SEBS and the prepared coupling agent ethanol solution in a high-speed mixer for 3-8 minutes at 50-70 ℃;
(4) and (3) putting the materials obtained in the steps (2) and (3), 13 g of SEBS-g-MAH and 2 g of antioxidant 1010 in a double-screw extruder, and performing melt extrusion and granulation.
Wherein, the length-diameter ratio of the screws of all the double-screw extruders is 48: 1, extruding and granulating in a double-screw extruder with nine zones for controlling temperature, wherein the processing temperature in one zone to nine zones is as follows in sequence: 185 ℃, 191 ℃, 187 ℃, 190 ℃, 193 ℃, 197 ℃, 192 ℃, 195 ℃, 198 ℃, 202 ℃ of the head, 28-38 HZ of the host frequency, 22-28 HZ of the feeding frequency, 2.9-3.8 MPa of the melt pressure, 0.03-0.06 MPa of the vacuum degree and 370-470 rpm of the granulator.
Example 4
The plant composite fiber filled polypropylene composite material comprises the following components:
(1) preparing 5.4 g of silane coupling agent KH560 into an ethanol solution containing 1-3 wt% of coupling agent; adding 108 g of straw powder, 39.6 g of bamboo powder, 32.4 g of wood powder and 270 g of prepared coupling agent ethanol solution into a high-speed stirrer for mixing, gradually adding 36 g of solution containing 1% of epoxy resin and 3% of graphene (the epoxy resin is uncured resin, the solvent is butanol, cyclohexanone or absolute ethyl alcohol and the like can be used as an alternative), continuously stirring for 30 minutes at 85 ℃, and drying to obtain graphene-coated plant powder filler; the particle size range of the graphene coated plant powder filler is 15-110 micrometers;
(2) carrying out melt blending on graphene-coated plant powder filler and 360 g of polyester resin, dissolving the blend by 2160 g of dimethylformamide solvent, and then spinning and drying to form composite fiber; grinding the composite fibers in a ball mill to prepare plant composite fiber powder, wherein the length range of the plant composite fiber powder is 22-285 micrometers, and the length-diameter ratio is 130: 1-240: 1;
(3) preparing 0.6 g of silane coupling agent KH560 into 1-3 wt% of coupling agent ethanol solution, and mixing 20 g of hollow glass microspheres, 580 g of co-polypropylene, 140 g of homo-polypropylene, 42 g of POE and the prepared coupling agent ethanol solution in a high-speed mixer for 3-8 minutes at the temperature of 50-70 ℃;
(4) and (3) putting the materials obtained in the steps (2) and (3), 30 g of POE-g-MAH and 2 g of antioxidant 1010 in a double-screw extruder, and performing melt extrusion and granulation.
Wherein, the length-diameter ratio of the screws of all the double-screw extruders is 48: 1, extruding and granulating in a double-screw extruder with nine zones for controlling temperature, wherein the processing temperature in one zone to nine zones is as follows in sequence: 185 ℃, 191 ℃, 187 ℃, 190 ℃, 193 ℃, 197 ℃, 192 ℃, 195 ℃, 198 ℃, 202 ℃ of the head, 28-38 HZ of the host frequency, 22-28 HZ of the feeding frequency, 2.9-3.8 MPa of the melt pressure, 0.03-0.06 MPa of the vacuum degree and 370-470 rpm of the granulator.
Example 5
The plant composite fiber filled polypropylene composite material comprises the following components:
(1) 1.8 g of silane coupling agent KH560 is prepared into an ethanol solution containing 1-3 wt% of the coupling agent; adding 60 g of straw powder and 90 g of prepared ethanol solution of a coupling agent into a high-speed stirrer for mixing, gradually adding 12 g of solution containing 1% of epoxy resin and 3% of graphene (the epoxy resin is uncured resin, the solvent is butanol, cyclohexanone or absolute ethanol can be used as well, and the like), continuously stirring for 30 minutes at 85 ℃, and drying to obtain graphene-coated plant powder filler; the particle size range of the graphene coated plant powder filler is 15-110 micrometers;
(2) carrying out melt blending on graphene-coated plant powder filler and 120 g of polyester resin, dissolving the blend by using 720 g of dimethylformamide solvent, and then spinning and drying to form composite fibers; grinding the composite fibers in a ball mill to prepare plant composite fiber powder, wherein the length range of the plant composite fiber powder is 22-285 micrometers, and the length-diameter ratio is 130: 1-240: 1;
(3) 1.2 g of silane coupling agent KH560 is prepared into 1-3 wt% of coupling agent ethanol solution, and 40 g of hollow glass beads, 660 g of polypropylene copolymer, 180 g of polypropylene homopolymer, 45 g of SBS and the prepared coupling agent ethanol solution are mixed in a high-speed mixer for 3-8 minutes at the temperature of 50-70 ℃;
(4) and (3) putting the materials obtained in the steps (2) and (3), 10 g of PP-g-MAH and 2 g of antioxidant 1010 in a double-screw extruder, and performing melt extrusion and granulation.
Wherein, the length-diameter ratio of the screws of all the double-screw extruders is 48: 1, extruding and granulating in a double-screw extruder with nine zones for controlling temperature, wherein the processing temperature in one zone to nine zones is as follows in sequence: 185 ℃, 191 ℃, 187 ℃, 190 ℃, 193 ℃, 197 ℃, 192 ℃, 195 ℃, 198 ℃, 202 ℃ of the head, 28-38 HZ of the host frequency, 22-28 HZ of the feeding frequency, 2.9-3.8 MPa of the melt pressure, 0.03-0.06 MPa of the vacuum degree and 370-470 rpm of the granulator.
The prepared composite materials were subjected to performance tests, and the results are shown in table 1.
The methods for performing various performance tests on the samples prepared in examples 1-5 above were as follows:
the specific gravity is measured according to ASTM D792 standard;
shrinkage (MD) was measured according to ASTM D995;
the melt index was measured according to ASTM D1238(230 ℃/2.16 kg);
the Rockwell hardness is measured according to ASTM D785;
the tensile strength and the elongation at break are measured according to the ASTM D638 standard;
flexural strength and flexural modulus were measured according to ASTM D790;
the notched impact strength of the cantilever beam is detected according to the ASTM D256 standard;
the heat distortion temperature is detected according to the ASTM D648 standard;
fog requirements, odor requirements, aldehyde ketone material requirements and VOC test values are tested according to the BT/SGMWJ0872-2016 standard.
TABLE 1 Properties of the composites prepared in the examples and comparison
As can be seen from Table 1, the density was controlled to be less than 0.93g/cm3 when the sum of the plant powder and the inorganic mineral filler was not more than 10%. The density is controlled at 0.99g/cm when the total content of the plant powder and the inorganic mineral filler is not more than 20%3The following. The plant fiber powder is ideal for controlling the density control of the polypropylene composite material. The plant fiber powder with a certain length-diameter ratio is beneficial to improving the bending strength and the bending modulus of the composite material, and the hollow glass beads are greatly helpful to increasing the melt index. The plant fiber powder and the hollow glass beads are matched for use, and the plant fiber powder and the hollow glass beads are very ideal for controlling the fog of the polypropylene composite material odor through the synergistic effect of different forms and sizes.
Claims (9)
1. The plant composite fiber filled polypropylene composite material is characterized by comprising the following raw materials in percentage by weight: 42-64% of copolymerized polypropylene, 6-18% of homopolymerized polypropylene, 5-18% of plant powder, 0-5% of inorganic mineral filler, 1-5% of elastomer, 0.8-3% of compatibilizer, 0.2-0.6% of coupling agent, 0.1-0.3% of antioxidant, 10-28% of polyester resin, 0.01-0.03% of epoxy resin and 0.03-0.08% of graphene;
the preparation method of the plant composite fiber filled polypropylene composite material comprises the following steps
(1) Adding plant powder and an ethanol solution containing 1-3 wt% of a coupling agent into a high-speed stirrer for mixing, gradually adding a solution containing 1% of epoxy resin and 3% of graphene, continuously stirring for 30 minutes at 85 ℃, and drying to obtain a graphene-coated plant powder filler, wherein the particle size range of the graphene-coated plant powder filler is 15-110 micrometers;
(2) carrying out melt blending on graphene-coated plant powder filler and polyester resin, dissolving the blend with a dimethylformamide solvent, spinning and drying to form composite fibers, and grinding the composite fibers in a ball mill to prepare plant composite fiber powder, wherein the length range of the plant composite fiber powder is 22-285 microns, and the length-diameter ratio is 130: 1-240: 1;
(3) when inorganic mineral fillers exist in the raw materials, mixing the inorganic mineral fillers, polypropylene and elastomer with an ethanol solution containing 1-3 wt% of a coupling agent in a high-speed mixer for 3-8 minutes at the temperature of 50-70 ℃; when the raw materials do not contain inorganic mineral fillers, mixing the polypropylene and the elastomer in a high-speed mixer for 3-8 minutes at the temperature of 50-70 ℃;
(4) and (3) placing the materials obtained in the steps (2) and (3), the compatibilizer and the antioxidant in a double-screw extruder, and performing melt extrusion and granulation.
2. The plant composite fiber-filled polypropylene composite material according to claim 1, wherein: the plant powder is at least one of straw powder, bamboo powder and wood powder.
3. The plant composite fiber-filled polypropylene composite material according to claim 1, wherein: the inorganic mineral filler is hollow glass beads, the average particle size is 0.8-85 micrometers, and the specific surface area is 9-17 m2/g。
4. The plant composite fiber-filled polypropylene composite material according to claim 1, wherein: the elastomer is at least one of POE, EPDM, SBS and SEBS.
5. The plant composite fiber-filled polypropylene composite material according to claim 1, wherein: the compatibilizer is at least one of SEBS-g-MAH, PP-g-MAH and POE-g-MAH.
6. The plant composite fiber-filled polypropylene composite material according to claim 1, wherein: the coupling agent is a silane coupling agent KH560, and the antioxidant is antioxidant 1010.
7. The preparation method of the plant composite fiber filled polypropylene composite material according to claim 1, wherein the plant composite fiber filled polypropylene composite material comprises the following steps: in the step (1), the dosage of the coupling agent is 3 percent of the total weight of the plant powder; in the step (3), the dosage of the coupling agent is 3 percent of the total weight of the inorganic mineral filler.
8. The method for preparing the plant composite fiber filled polypropylene composite material according to claim 1, wherein the ratio of the plant powder to the solution in the step (1) is 5: 1.
9. the preparation method of the plant composite fiber filled polypropylene composite material according to claim 1, wherein the graphene-coated plant powder filler in the step (2) is prepared by the following steps in percentage by weight: polyester resin: dimethylformamide solvent is 1: 2: 12.
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| CN111961284A (en) * | 2020-08-26 | 2020-11-20 | 安徽国泰智能科技有限公司 | Light high-strength air guide sleeve for light truck |
| CN112111105A (en) * | 2020-08-28 | 2020-12-22 | 安徽越洋达新能源科技有限公司 | High strength power support |
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| CN100999610A (en) * | 2006-01-12 | 2007-07-18 | 中国林业科学研究院木材工业研究所 | Wood plastic composite material composection and formed board thereof and their preparation process |
| CN103571038A (en) * | 2012-07-20 | 2014-02-12 | 上海杰事杰新材料(集团)股份有限公司 | Nature fiber reinforced thermoplastic resin unidirectional prepreg tape and preparation method thereof |
| CN105585868A (en) * | 2015-12-21 | 2016-05-18 | 南京聚锋新材料有限公司 | Straw-plastic composite and preparation method thereof |
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