CN110964251A - Modified natural fiber reinforced polypropylene composite material and preparation method thereof - Google Patents
Modified natural fiber reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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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
- C08L23/12—Polypropene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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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
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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
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Abstract
The invention discloses a modified natural fiber reinforced polypropylene composite material and a preparation method thereof, wherein the composite material is prepared from 75-84 parts of polypropylene, 15-20 parts of modified natural fiber, 0.5-1 part of initiator, 1-5 parts of cardanol, 0.2-0.4 part of antioxidant, 0.5-1 part of lubricant and 0-2 parts of other auxiliary agents. According to the invention, through surface modification of natural fibers, under the action of an initiator and cardanol, the hydrophobicity of the natural fibers is obviously improved, the interface bonding force between the fibers and a polypropylene chain segment is improved, and the mechanical property of polypropylene is effectively improved. The modified natural fiber reinforced polypropylene composite material prepared by the invention has the excellent performances of small density, high impact and high modulus, can be popularized on parts such as automobile door trim panels, luggage compartment ornaments and seat back plates, and has wide prospects in the field of automobiles.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a modified natural fiber reinforced polypropylene composite material and a preparation method thereof.
Background
With the rapid development of automobile technology, the number of automobiles is rapidly increased, a large amount of petrochemical fuel is consumed, the pollution degree of the environment is increased, the problems of environmental deterioration, resource shortage and the like are increasingly prominent, and the main trend of the development of the automobile industry is energy conservation, environmental protection, safety and light weight. Statistics shows that the fuel consumption can be reduced by 6-8% when the weight of the automobile is reduced by 10%. The light weight of the automobile becomes one of the important trends in the development of the automobile industry, and the selection of high-performance light materials is an effective measure. The high-performance fiber reinforced polypropylene composite material has the characteristics of high specific strength, high modulus, low density, corrosion resistance and the like, and becomes a light material which is focused in the field of automobile industry. The glass fiber reinforced composite material is the most common material with the widest application range, but the preparation process of the glass fiber needs to consume a large amount of resources, the obtained composite material is difficult to recycle, seriously pollutes the ecological environment, and does not meet the requirement of green sustainable development. The fibrilia belongs to one of natural plant fibers, has the advantages of wide source, low cost, reproducibility, degradability, environmental friendliness, low density and the like, and the prepared fibrilia composite material has low density, recoverability, good sound insulation performance and excellent impact resistance, and is mainly applied to automobile interior structural materials, such as automobile door interior trim panels, luggage compartment decorations, seat back panels and the like. However, the fibrilia surface contains a large amount of polar hydrophilic matrixes, has strong hydrophilicity and poor compatibility with a polypropylene nonpolar chain segment, reduces the performance of the composite material, and limits the application of the fibrilia reinforced composite material, so that the development of a plant fiber reinforced polypropylene micro-foaming material with large rigidity, high strength and small density becomes an urgent need in the automobile lightweight technology, just conforms to the development trend of automobiles, and has a wide development prospect on automobiles.
Disclosure of Invention
The invention aims to solve the problems that the surface of natural plant fiber contains polar groups, has strong hydrophilicity, poor compatibility with non-polar polypropylene, difficult dispersion in a matrix, influence on the comprehensive performance of a fiber composite material and the like, and provides a modified natural fiber reinforced polypropylene composite material and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
the modified natural fiber reinforced polypropylene composite material is prepared from the following components in parts by weight:
the modified natural fiber is obtained by modifying the surface of long fibrilia by a coupling agent, and the preparation method comprises the following steps: weighing 90-96 parts of long fibrilia, adding the long fibrilia into acetone, soaking at room temperature for 10-30min, adding 4-10 parts of a coupling agent, uniformly stirring, soaking for 24-48 h, washing with acetone for 3-5 times, and vacuum drying the product at 50-80 ℃ for 24-48 h to obtain the modified natural fiber.
In a further scheme, the polypropylene is at least one of homo-polypropylene, block copolymerization polypropylene and random copolymerization polypropylene.
The long fibrilia is long fibrilia woven by 3-7 double-ply yarns, for example, 4 double-ply yarns; the coupling agent is at least one of 3-isocyanate propyl methyl dimethoxy silane, 3-isocyanate propyl triethoxy silane and 3-isocyanate propyl trimethoxy silane.
Preferably, the solid content of the cardanol is 99.25-99.45%.
The initiator is at least one of dibenzoyl peroxide and azobisisobutyronitrile.
The antioxidant is selected from at least one of hindered phenol antioxidant, thiosulfate antioxidant and phosphite antioxidant; the hindered phenol antioxidant is an antioxidant 1010, the thiosulfate antioxidant is an antioxidant DLTP, and the phosphite antioxidant is an antioxidant 168.
The lubricant is at least one of calcium stearate and zinc stearate.
The other auxiliary agent is at least one of ultraviolet absorbent, surface brightener, light stabilizer, antistatic agent and colorant.
The invention also aims to provide a preparation method of the modified natural fiber reinforced polypropylene composite material, which comprises the following steps:
(1) weighing 90-96 parts of long fibrilia, adding the long fibrilia into acetone, soaking at room temperature for 10-30min, adding 4-10 parts of a coupling agent, uniformly stirring, soaking for 24-48 h, washing with acetone for 3-5 times, and vacuum drying the product at 50-80 ℃ for 24-48 h to obtain modified natural fiber;
(2) mixing 75-84 parts of polypropylene, 0.5-1 part of initiator, 1-5 parts of cardanol, 0.2-0.4 part of antioxidant, 0.5-1 part of lubricant and 0-2 parts of other auxiliary agents in a high-speed mixer for 10min, putting into a main feed of a co-rotating double-screw extruder, simultaneously weighing 15-20 parts of modified long fibrilia prepared in the step (1), adding the modified long fibrilia through a glass fiber port, and performing melt extrusion granulation to prepare the low-density high-modulus polypropylene long fibrilia composite material; wherein the extrusion temperature of the extruder is 170-190 ℃, the rotating speed of the screw is 350-400 r/min, and the vacuum degree is-0.06-0.08 MPa.
The invention has the beneficial effects that:
the cardanol is a natural compound refined by processing cashew shells, belongs to a phenol derivative, and is structurally characterized in that a long side carbon chain with 15 carbon atoms of unsaturation is arranged at the meta position of phenol, so that addition and polymerization reactions are easy to occur with a polymer, the polymer can be chemically modified, and in addition, phenolic hydroxyl groups have certain activity.
The surface of the long fibrilia contains abundant hydroxyl, the surface polarity is high, and the compatibility with polypropylene is poor. The surface of the fiber is modified by adopting an isocyanate type coupling agent, the hydroxyl on the surface of the cellulose and silanol are subjected to chemical reaction, and the fiber is subjected to polycondensation on the surface of the fibrilia to form a mold, so that the structural form that organic groups face outwards is formed, the plant fiber is changed from hydrophilicity to hydrophobicity, and meanwhile, the surface also has active isocyanate groups, and the fiber is prepared for further reaction.
In the processing process of the material, the initiator is thermally decomposed to generate a primary free radical, a tertiary carbon atom of polypropylene is initiated to form a free radical, a side chain double bond of cardanol is also initiated to form a cardanol free radical, the free radicals collide with each other, a long-chain alkyl of the cardanol is grafted to a polypropylene chain segment, and a phenolic hydroxyl group at the other end is grafted with an isocyanate group grafted on the surface of long fibrilia, so that the resin matrix can effectively coat the long fibrilia, the interface bonding force of resin and fiber is increased, and the mechanical strength of the material is effectively improved.
The density of the modified natural fiber reinforced polypropylene composite material prepared by the invention can be as low as 0.98g/cm under the condition that the modulus is equivalent to that of chopped glass fiber reinforced polypropylene3The high-impact-resistance glass fiber reinforced polypropylene composite material has low density, high impact and high modulus, can be widely applied to automotive door trim panels, luggage compartment ornaments, seat back panels and the like, can replace glass fiber reinforced polypropylene materials, and has wide prospects in the automotive field.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the specific embodiments illustrated. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
The reagents used in the following examples and comparative examples are all commercially available products. The model and supplier of the reagents were as follows: the block copolymerization polypropylene is Yanshan petrochemical K9015, the random copolymerization polypropylene is Yanshan petrochemical K4220 and the homopolymerization polypropylene is Yanshan petrochemical K1215, and the reagents are used for explaining the sources and components of the reagents used in the experiment of the invention so as to be fully disclosed, and the invention cannot be realized by adopting other similar reagents or reagents provided by other suppliers.
Example 1
The modified natural fiber reinforced polypropylene composite material in the embodiment is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps:
(1) weighing 96 parts of long fibrilia, adding the long fibrilia into acetone, soaking at room temperature for 30min, slowly adding 4 parts of 3-isocyanate propyl methyl dimethoxy silane, uniformly stirring, soaking for 24h, washing for 3 times with acetone, and vacuum drying the product at 50 ℃ for 24h to obtain the modified long fibrilia;
(2) mixing 84 parts of homopolymerized polypropylene, 0.5 part of dibenzoyl peroxide, 1 part of cardanol, 0.2 part of antioxidant 1010 and 0.5 part of calcium stearate in a high-speed mixer for 10min, putting into a main feed of a co-rotating double-screw extruder, simultaneously weighing 15 parts of modified long fibrilia prepared in the step (1), adding through a glass fiber port, and performing melt extrusion granulation to obtain a polypropylene composite material; wherein the extrusion temperature of the extruder is 170 ℃, the rotating speed of the screw is 350r/min, and the vacuum degree is-0.06 MPa.
Example 2
The modified natural fiber reinforced polypropylene composite material in the embodiment is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps:
(1) weighing 90 parts of long fibrilia, adding the long fibrilia into acetone, soaking at room temperature for 10min, slowly adding 10 parts of 3-isocyanate propyl triethoxysilane, uniformly stirring, soaking for 48h, washing with acetone for 5 times, and vacuum drying the product at 80 ℃ for 48h to obtain modified long fibrilia;
(2) mixing 52 parts of homopolymerized polypropylene, 30 parts of random copolymerization polypropylene, 1 part of azobisisobutyronitrile, 3 parts of cardanol, 0.2 part of antioxidant 1010, 0.2 part of antioxidant DLTP and 1 part of calcium stearate in a high-speed mixer for 10min, putting into a main feed of a co-rotating double-screw extruder, simultaneously weighing 15 parts of modified long fibrilia prepared in the step (1), adding through a glass fiber port, and performing melt extrusion granulation to prepare the polypropylene composite material; wherein the extrusion temperature of the extruder is 190 ℃, the rotating speed of the screw is 400r/min, and the vacuum degree is-0.08 MPa.
Example 3
The modified natural fiber reinforced polypropylene composite material in the embodiment is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps:
(1) weighing 95 parts of long fibrilia, adding the long fibrilia into acetone, soaking at room temperature for 10min, slowly adding 10 parts of 3-isocyanate propyl triethoxysilane, uniformly stirring, soaking for 48h, washing with acetone for 5 times, and vacuum drying the product at 80 ℃ for 48h to obtain modified long fibrilia;
(2) mixing 45 parts of homopolymerized polypropylene, 30 parts of block copolymerization polypropylene, 0.75 part of dibenzoyl peroxide, 5 parts of cardanol, 0.2 part of antioxidant 1010, 0.2 part of antioxidant 168, 1 part of calcium stearate, 0.5 part of UV-P, 0.5 part of benzophenone and 1 part of black master batch in a high-speed mixer for 10min, putting into a main feed of a co-rotating double-screw extruder, simultaneously weighing 20 parts of the modified long hemp fiber prepared in the step (1), adding the fiber through a glass fiber port, and performing melt extrusion granulation to prepare a polypropylene composite material; wherein the extrusion temperature of the extruder is 180 ℃, the rotating speed of the screw is 375r/min, and the vacuum degree is-0.07 MPa.
Example 4
The modified natural fiber reinforced polypropylene composite material in the embodiment is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps:
(1) weighing 92 parts of long fibrilia, adding the long fibrilia into acetone, soaking at room temperature for 10-30min, slowly adding 8 parts of 3-isocyanate propyl methyl dimethoxy silane, uniformly stirring, soaking for 36h, washing with acetone for 5 times, and vacuum drying the product at 80 ℃ for 48h to obtain the modified long fibrilia;
(2) mixing 47 parts of block copolymer polypropylene, 30 parts of random copolymer polypropylene, 0.75 part of dibenzoyl peroxide, 3 parts of cardanol, 0.1 part of antioxidant 1010, 0.1 part of antioxidant 168 and 0.75 part of calcium stearate in a high-speed mixer for 10min, putting into a main feed of a co-rotating double-screw extruder, simultaneously weighing 20 parts of the modified long fibrilia prepared in the step (1), adding through a fiber opening, and performing melt extrusion granulation to obtain a polypropylene composite material; wherein the extrusion temperature of the extruder is 180 ℃, the rotating speed of the screw is 400r/min, and the vacuum degree is-0.08 MPa.
Comparative example 1
The glass fiber reinforced polypropylene composite material in the comparative example is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps:
mixing 77 parts of homopolymerized polypropylene, 3 parts of polypropylene grafted maleic anhydride, 0.15 part of antioxidant 1010, 0.15 part of antioxidant 168 and 0.75 part of calcium stearate in a high-speed mixer for 10min, putting into a main feed of a co-rotating double-screw extruder, simultaneously weighing 20 parts of chopped glass fiber, adding from a side feed hopper, and carrying out melt extrusion and granulation to obtain a polypropylene composite material; wherein the extrusion temperature of the extruder is 210 ℃, the rotating speed of the screw is 400r/min, and the vacuum degree is-0.06 MPa.
The main physical property indexes of the polypropylene composite materials prepared in the above examples 1 to 3 and comparative example 1 are measured according to the related test standards, and the test standards and test results of the melt flow rate, the density, the tensile strength, the notch impact strength of the simply supported beam, the bending strength and the bending modulus are shown in the following table 1.
Table 1: main physical property indexes of fiber reinforced polypropylene composite materials of examples 1-3 and comparative example 1
Note: the conditions for the above test and the dimensions of the test bars are as follows:
the sample bar used for the tensile strength test has the length of 170mm, the width of the end part of 20mm, the width of the narrow edge of 10mm and the tensile rate of 50 mm/min;
the sample bar used for the bending strength test has the size of 80mm in length, 10mm in width, 4mm in thickness and 2mm/min in bending rate;
the sample bar used for the flexural modulus test has the dimensions of 80mm in length, 10mm in width, 4mm in thickness and 2mm/min in bending rate;
the sample bar used for the notch impact strength of the cantilever beam has the size of 80mm in length, 10mm in width and 4mm in thickness.
If functional additives such as ultraviolet light absorbers, light stabilizers, antistatic agents, coloring agents and the like are added into the preparation components, the composite material has corresponding characteristics and is also protected by the invention.
Compared with the prior art, the invention has the following advantages:
it can be seen from table 1 that after the long fibrilia is modified, the hydrophobicity of the long fibrilia is obviously improved under the action of the initiator and the cardanol, the interface bonding force between the fiber and the polypropylene chain segment is improved, and the mechanical property of the polypropylene is effectively improved.
The polypropylene long fibrilia composite material prepared by the invention has the advantages of low density, high impact and high modulus, the performance is close to that of a glass fiber reinforced polypropylene composite material, but the density is lower than that of glass fiber with the same content, so the polypropylene long fibrilia composite material can replace the existing glass fiber reinforced polypropylene material, can be popularized on parts such as automobile door interior trimming panels, luggage compartment ornaments, seat back plates and the like, and has wide prospect in the field of automobiles.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications can be made to the embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make modifications and alterations without departing from the scope of the present invention.
Claims (9)
1. The modified natural fiber reinforced polypropylene composite material is characterized by being prepared from the following components in parts by weight:
the modified natural fiber is obtained by modifying the surface of long fibrilia by a coupling agent, and the preparation method comprises the following steps: weighing 90-96 parts of long fibrilia, adding the long fibrilia into acetone, soaking at room temperature for 10-30min, adding 4-10 parts of a coupling agent, uniformly stirring, soaking for 24-48 h, washing with acetone for 3-5 times, and vacuum drying the product at 50-80 ℃ for 24-48 h to obtain the modified natural fiber.
2. The modified natural fiber reinforced polypropylene composite of claim 1, wherein the polypropylene is at least one of homo polypropylene, block co-polypropylene, random co-polypropylene.
3. The modified natural fiber reinforced polypropylene composite material of claim 1, wherein the long fibrilia is long fibrilia woven by 3-7 double-ply yarns, and the coupling agent is at least one of 3-isocyanatopropyl methyl dimethoxy silane, 3-isocyanatopropyl triethoxy silane and 3-isocyanatopropyl trimethoxy silane.
4. The modified natural fiber reinforced polypropylene composite material of claim 1, wherein the cardanol has a solid content of 99.25 to 99.45%.
5. The modified natural fiber reinforced polypropylene composite of claim 1, wherein the initiator is at least one of dibenzoyl peroxide and azobisisobutyronitrile.
6. The modified natural fiber reinforced polypropylene composite of claim 1, wherein the antioxidant is at least one selected from hindered phenolic antioxidants, thiosulfate antioxidants, phosphite antioxidants;
the hindered phenol antioxidant is an antioxidant 1010, the thiosulfate antioxidant is an antioxidant DLTP, and the phosphite antioxidant is an antioxidant 168.
7. The modified natural fiber reinforced polypropylene composite of claim 1, wherein the lubricant is at least one of calcium stearate and zinc stearate.
8. The modified natural fiber reinforced polypropylene composite of claim 1, wherein the other auxiliary agent is at least one of an ultraviolet absorber, a surface brightener, a light stabilizer, an antistatic agent, and a colorant.
9. A method for preparing a polypropylene composite according to any one of claims 1 to 8, comprising the steps of:
(1) weighing 90-96 parts of long fibrilia, adding the long fibrilia into acetone, soaking at room temperature for 10-30min, adding 4-10 parts of a coupling agent, uniformly stirring, soaking for 24-48 h, washing with acetone for 3-5 times, and vacuum drying the product at 50-80 ℃ for 24-48 h to obtain modified natural fiber;
(2) mixing 75-84 parts of polypropylene, 0.5-1 part of initiator, 1-5 parts of cardanol, 0.2-0.4 part of antioxidant, 0.5-1 part of lubricant and 0-2 parts of other auxiliary agents in a high-speed mixer for 10min, putting into a main feed of a co-rotating double-screw extruder, simultaneously weighing 15-20 parts of modified natural fiber prepared in the step (1), adding through a glass fiber port, and performing melt extrusion granulation to prepare the low-density high-modulus polypropylene long-fibrilia composite material; wherein the extrusion temperature of the extruder is 170-190 ℃, the rotating speed of the screw is 350-400 r/min, and the vacuum degree is-0.06-0.08 MPa.
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| CN2018115452692 | 2018-12-17 | ||
| CN201811545269.2A CN109749234A (en) | 2018-12-17 | 2018-12-17 | A kind of long flaxen fiber composite material and preparation method of low-density high modulus polypropylene |
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| CN114702784A (en) * | 2022-04-12 | 2022-07-05 | 中南林业科技大学 | Natural fiber reinforced epoxy resin composite material, preparation method thereof and application thereof in 3D printing |
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| CN110452307B (en) * | 2019-07-24 | 2021-05-11 | 衢州学院 | Modified nano-cellulose and preparation method thereof |
| CN116769270B (en) * | 2023-06-25 | 2024-03-08 | 广东丙辛新材料有限公司 | Low-density high-pressure polyethylene closed-cell foam plastic plate and production process thereof |
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