CN112608553A - Plant fiber reinforced polypropylene composite material and preparation method thereof - Google Patents
Plant fiber reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a plant fiber reinforced polypropylene composite material which is prepared from the following raw materials in parts by weight: 45-75 parts of polypropylene, 20-50 parts of plant fiber, 0.1-1 part of organic peroxide, 1-12 parts of itaconic acid diglycidyl ester, 0.1-3 parts of lubricant and 0.1-2 parts of antioxidant, wherein the average length of the plant fiber is 3-40 mm. The invention adopts the itaconic acid diglycidyl ester derived from renewable resources as the coupling agent, which can form a bridge function between the plant fiber and the polypropylene under the action of the organic peroxide, thereby obviously improving the interface bonding force between the plant fiber and the polypropylene. The plant fiber reinforced polypropylene composite material prepared by the invention has the advantages of high strength, good toughness, light weight, low cost and the like, and the preparation process is simple, the production efficiency is high, the industrial production is easy, and the development prospect is wide.
Description
Technical Field
The invention relates to the field of plastic modification and plant fiber comprehensive utilization, in particular to a plant fiber reinforced polypropylene composite material and a preparation method thereof.
Background
The plant fiber has the advantages of light weight, high specific strength, low cost, rich reserves and the like. Furthermore, they are all derived from renewable resources, being able to degrade under natural conditions without any harm to the environment. The plant fiber is used as the filler, and the degradable high-performance plant fiber reinforced polypropylene composite material is developed, so that the production cost of the composite material can be obviously reduced, great economic benefits are brought to enterprises, the environmental pressure can be relieved, great social benefits are generated, and the degradable high-performance plant fiber reinforced polypropylene composite material is a green, low-carbon and recyclable material with great development prospect.
When the plant fiber reinforced polypropylene composite material is prepared, the plant fiber surface contains a large amount of hydroxyl groups to show strong hydrophilicity, and the polypropylene is a typical hydrophobic polymer, so that the compatibility of the plant fiber surface and the polypropylene is poor, the interfacial bonding force between the plant fiber and the polypropylene matrix is weak, and the composite material with excellent mechanical property is difficult to obtain. Therefore, improving the compatibility between the plant fiber and the polypropylene matrix is a key technology for preparing the high-performance plant fiber reinforced polypropylene composite material.
Chinese patent application publication No. CN104693606A discloses a plant fiber reinforced polypropylene composite material, a preparation method thereof, and an application thereof in preparing automobile parts. The patent uses small-molecule vegetable oil as a compatilizer, however, vegetable oil which is typical hydrophobic grease has difficulty in generating good interaction with hydrophilic vegetable fibers. In addition, the chemical structure of the vegetable oil does not have reactive functional groups, and the vegetable oil is easy to exude from the polypropylene matrix, thereby affecting the comprehensive performance of the material.
Chinese patent application publication No. CN102585358 discloses a natural fiber reinforced polypropylene composite material and a preparation method thereof. The patent firstly uses alkali liquor to treat natural fibers to obtain natural fibers with rough surfaces, and then uses graft polymers of polar monomers as compatilizers to improve the interface bonding force between the natural fibers and polypropylene. Although this technique can improve the mechanical properties of natural fiber-reinforced polypropylene composites, the van der waals forces act between the graft polymer of the polar monomer and the natural fibers and polypropylene alone, making it difficult to obtain high-performance composites. In addition, the strength of the natural fiber itself is significantly reduced by the alkali treatment.
Chinese patent application publication No. CN102382374A discloses a fiber reinforced polypropylene automotive interior material and a preparation method thereof. The patent adopts gamma-glycidoxypropyltrimethoxysilane (KH560) as a coupling agent to treat plant fibers, improves the interfacial compatibility of plant fiber reinforced polypropylene to a certain extent, but the use of the coupling agent does not consider the relevant action with a polypropylene matrix, and has a larger space for improving the mechanical property.
Disclosure of Invention
The invention aims to provide a plant fiber reinforced polypropylene composite material with excellent mechanical property.
A plant fiber reinforced polypropylene composite material is prepared from the following raw materials in parts by weight:
wherein, the epoxy compound is an unsaturated epoxy compound derived from renewable resources, and the chemical structure of the epoxy compound is as shown in formula I:
the itaconic acid diglycidyl ester has the functions of a coupling agent and a toughening agent, can obviously improve the interface bonding force between the plant fiber and the polypropylene, and can obviously improve the impact strength of the plant fiber reinforced polypropylene composite material. The dosage of the itaconic acid diglycidyl ester directly influences the compatibility of the plant fiber and the polypropylene and the mechanical property of the composite material thereof. If the dosage of the itaconic acid diglycidyl ester is too small, the effect of improving the compatibility of the plant fiber and the polypropylene cannot be fully exerted, the toughness of the composite material is influenced, and the impact strength is reduced; if the amount of the free itaconic acid diglycidyl ester is too large, the rest free itaconic acid diglycidyl ester is dispersed in the polypropylene matrix in the form of small droplets, and the strength and the modulus of the plant fiber reinforced polypropylene composite material are finally reduced. With the change of the dosage of the itaconic acid diglycidyl ester, other raw materials are also adjusted in a suitable dosage, and preferably, the plant fiber reinforced polypropylene composite material is prepared from the following raw materials in parts by weight:
the polypropylene is one or the combination of two of homopolymerized polypropylene or random copolymer of propylene and ethylene.
The melt index of the polypropylene is 5-50 g/10min, preferably 20-50 g/10min, and the polypropylene resin with higher melt index is selected to be beneficial to the uniform dispersion of plant fibers in the matrix resin.
The plant fiber comprises kenaf fiber, jute fiber, flax fiber, hemp fiber, sisal fiber, hemp fiber, ramie fiber, palm fiber or coconut shell fiber. The plant fibers in the present invention act to increase the strength and modulus of the plant fiber reinforced polypropylene composite, similar to the "rebar" in reinforced concrete.
The average length of the plant fiber is 3-40 mm.
The organic peroxide is one or a mixture of more of benzoyl peroxide, dicumyl peroxide, di-tert-butyl peroxide, lauroyl peroxide and 2-butanone peroxide.
The lubricant is one or a mixture of more than two of polyethylene wax, polypropylene wax, polytetrafluoroethylene, butyl stearate, oleamide, erucamide or stearamide. Such lubricants can significantly enhance the processability of plant fiber reinforced polypropylene composites, particularly when the plant fiber loading is high, and it is particularly desirable to increase the melt flow of the composite by adding a lubricant.
The antioxidant is prepared by compounding hindered phenol antioxidant and phosphite antioxidant according to the weight ratio of 1: 1.
The invention also provides a preparation method of the plant fiber reinforced polypropylene composite material, which comprises the following steps:
uniformly mixing polypropylene, plant fiber, organic peroxide, itaconic acid diglycidyl ester, a lubricant and an antioxidant by using a high-speed mixer, and then carrying out melt blending extrusion, bracing, cooling and granulation by using a double-screw extruder to obtain the plant fiber reinforced polypropylene composite material granules.
The length-diameter ratio of screws of the double-screw extruder is 30: 1-45: 1, and the melt blending temperature is 170-200 ℃.
The invention adopts itaconic acid diglycidyl ester as a coupling agent to improve the mechanical property of the plant fiber reinforced polypropylene composite material. On one hand, epoxy groups in the itaconic acid diglycidyl ester can perform coupling reaction with hydroxyl groups on the surface of the plant fiber; on the other hand, the unsaturated double bond contained in the polypropylene resin is subjected to a grafting reaction with the polypropylene matrix to form a covalent bond under the action of radicals generated by the organic peroxide. Therefore, the itaconic acid diglycidyl ester plays a good role of a bridge between the plant fiber and the polypropylene matrix through a covalent bond, and the high-performance plant fiber reinforced polypropylene composite material can be prepared.
In addition, the itaconic acid diglycidyl ester also has the effect of a toughening agent, the itaconic acid diglycidyl ester which does not have a grafting reaction with the polypropylene can be coupled on the surface of the plant fiber to form a layer of flexible interface phase, and the flexible interface phase in the plant fiber reinforced polypropylene composite material can absorb external energy under the action of external force, so that the toughness of the composite material is greatly improved.
The preparation method of the plant fiber reinforced polypropylene composite material mainly comprises the following steps of:
compared with the prior art, the invention has the following advantages and beneficial results:
the invention adopts the itaconic acid diglycidyl ester derived from renewable resources as the coupling agent of the plant fiber and the polypropylene, and the novel coupling agent can effectively improve the interface bonding force between the plant fiber and the polypropylene through forming covalent bonds respectively between the plant fiber and the polypropylene under the action of organic peroxide, thereby obtaining the plant fiber reinforced polypropylene composite material with high performance.
The plant fiber reinforced polypropylene composite material prepared by the double-screw extruder has the advantages of simple production process, high production efficiency and easy industrial production; and the plant fiber is not required to be treated by alkali liquor, and the environment is not polluted.
The plant fiber reinforced polypropylene composite material prepared by the invention has the advantages of high strength, good toughness, low cost, light weight and the like, is a novel green, low-carbon and recyclable composite material, and has very important significance for sustainable development economy.
Drawings
FIG. 1 is an SEM photograph of a 30% jute-reinforced polypropylene composite in example 2 of the present invention.
FIG. 2 is an SEM photograph of a 30% jute-reinforced polypropylene composite in comparative example 1 in accordance with the present invention.
Detailed Description
For further understanding of the present invention, the following will specifically describe a plant fiber reinforced polypropylene composite material and a method for preparing the same with reference to the following examples, but the present invention is not limited to these examples. The invention is not limited to the above embodiments, and those skilled in the art will recognize that many modifications and variations can be made in the process or formulation without departing from the spirit and scope of the invention.
Example 1
Weighing 72.6 parts of polypropylene (with the melt index of 11.2g/10min), 20 parts of jute fiber, 0.4 part of dicumyl peroxide, 4 parts of itaconic acid diglycidyl ester, 2 parts of lubricant (oleamide) and 1 part of antioxidant (the antioxidant 1010 and the antioxidant 168 are compounded in a ratio of 1: 1) according to the weight formula. Then adding the raw materials into a high-speed mixer for uniform mixing, then adding the mixed materials into a double-screw extruder for melt blending (the temperature of the double-screw extruder is 170 ℃, 175 ℃, 180 ℃, 185 ℃, 185 ℃, 190 ℃, 190 ℃, 190 ℃, 185 ℃ and 180 ℃ in sequence from a feed inlet to a machine head), and then drawing, air cooling and granulating to obtain the granules of the plant fiber reinforced polypropylene composite material. The length-diameter ratio of the screws of the twin-screw extruder in this example was 40: 1.
The obtained pellets were injection molded into a standard test sample bar in an injection molding machine, and mechanical properties were measured using a universal tester and a pendulum impact tester, and the mechanical property data are shown in table 1.
Example 2
Weighing 61.5 parts of polypropylene (with the melt index of 11.2g/10min), 30 parts of jute fiber, 0.5 part of dicumyl peroxide, 5 parts of itaconic acid diglycidyl ester, 2 parts of lubricant (stearic acid amide) and 1 part of antioxidant (the antioxidant 1010 and the antioxidant 168 are compounded according to the ratio of 1: 1). Then adding the raw materials into a high-speed mixer for uniform mixing, then adding the mixed materials into a double-screw extruder for melt blending (the temperature of the double-screw extruder is 170 ℃, 175 ℃, 180 ℃, 185 ℃, 185 ℃, 190 ℃, 190 ℃, 190 ℃, 185 ℃ and 180 ℃ in sequence from a feed inlet to a machine head), and then drawing, air cooling and granulating to obtain the granules of the plant fiber reinforced polypropylene composite material. The length-diameter ratio of the screws of the twin-screw extruder in this example was 40: 1.
The pellets obtained were injection molded in an injection molding machine into standard test specimens, the SEM photographs of which are shown in FIG. 1. As can be seen from fig. 1, after the organic peroxide and the diglycidyl itaconate are added to the hydrophilic plant fiber and the hydrophobic polypropylene, the combination between the hydrophilic plant fiber and the hydrophobic polypropylene is very tight, the plant fiber can be well wrapped by the polypropylene resin, and the interface between the hydrophilic plant fiber and the hydrophobic polypropylene has no gap, which indicates that the compatibility between the plant fiber and the polypropylene is significantly improved.
Mechanical property tests are carried out by using a universal testing machine and a pendulum impact testing machine, and the data of the mechanical property are shown in table 1.
Example 3
Weighing 49.4 parts of polypropylene (with the melt index of 11.2g/10min), 40 parts of jute fiber (with the average length of 100mm), 0.6 part of dicumyl peroxide, 6 parts of itaconic acid diglycidyl ester, 3 parts of lubricant (erucamide) and 1 part of antioxidant (antioxidant 1010 and antioxidant 168 are compounded in a ratio of 1: 1) according to the weight formula. Then adding the raw materials into a high-speed mixer, uniformly mixing, adding the mixed materials into a feeding hopper of a double-screw extruder, carrying out melt blending (the temperature of the double-screw extruder is 170 ℃, 175 ℃, 180 ℃, 180 ℃, 185 ℃, 185 ℃, 190 ℃, 190 ℃, 190 ℃, 185 ℃ and 180 ℃ in sequence from a feeding hole to a machine head), and then carrying out bracing, air cooling and granulation to obtain the granules of the plant fiber reinforced polypropylene composite material. The length-diameter ratio of the screws of the twin-screw extruder in this example was 40: 1.
The obtained pellets were injection molded into a standard test sample bar in an injection molding machine, and mechanical properties were measured using a universal tester and a pendulum impact tester, and the mechanical property data are shown in table 1.
Example 4
Weighing 37.2 parts of polypropylene (with the melt index of 11.2g/10min), 50 parts of jute fiber, 0.8 part of benzoyl peroxide, 8 parts of itaconic acid diglycidyl ester, 3 parts of lubricant (stearic acid amide) and 1 part of antioxidant (the antioxidant 1010 and the antioxidant 168 are compounded according to the weight ratio of 1: 1). Then adding the raw materials into a high-speed mixer for uniform mixing, then adding the mixed materials into a double-screw extruder for melt blending (the temperature of the double-screw extruder is 170 ℃, 175 ℃, 180 ℃, 185 ℃, 185 ℃, 190 ℃, 190 ℃, 190 ℃, 185 ℃ and 180 ℃ in sequence from a feed inlet to a machine head), and then drawing, air cooling and granulating to obtain the granules of the plant fiber reinforced polypropylene composite material. The length-diameter ratio of the screws of the twin-screw extruder in this example was 40: 1.
The obtained pellets were injection molded into a standard test sample bar in an injection molding machine, and mechanical properties were measured using a universal tester and a pendulum impact tester, and the mechanical property data are shown in table 1.
Comparative example 1
67 parts of polypropylene (with the melt index of 11.2g/10min), 30 parts of jute fiber, 2 parts of lubricant (oleamide) and 1 part of antioxidant (antioxidant 1010 and antioxidant 168 are compounded in a ratio of 1: 1) are weighed according to the weight formula. Then adding the raw materials into a high-speed mixer for uniform mixing, then adding the mixed materials into a double-screw extruder for melt blending (the temperature of the double-screw extruder is 170 ℃, 175 ℃, 180 ℃, 185 ℃, 185 ℃, 190 ℃, 190 ℃, 190 ℃, 185 ℃ and 180 ℃ in sequence from a feed inlet to a machine head), and then drawing, air cooling and granulating to obtain the granules of the plant fiber reinforced polypropylene composite material. The length-diameter ratio of the screws of the twin-screw extruder in this example was 40: 1.
The pellets obtained were injection molded in an injection molding machine into standard test specimens, the SEM photographs of which are shown in FIG. 2; mechanical property tests are carried out by using a universal testing machine and a pendulum impact testing machine, and the data of the mechanical property are shown in table 1.
Comparative example 2
63 parts of polypropylene (with the melt index of 11.2g/10min), 30 parts of jute fiber, 4 parts of itaconic acid diglycidyl ester, 2 parts of lubricant (oleamide) and 1 part of antioxidant (antioxidant 1010 and antioxidant 168 are compounded in a ratio of 1: 1) according to the weight formula. Then adding the raw materials into a high-speed mixer for uniform mixing, then adding the mixed materials into a double-screw extruder for melt blending (the temperature of the double-screw extruder is 170 ℃, 175 ℃, 180 ℃, 185 ℃, 185 ℃, 190 ℃, 190 ℃, 190 ℃, 185 ℃ and 180 ℃ in sequence from a feed inlet to a machine head), and then drawing, air cooling and granulating to obtain the granules of the plant fiber reinforced polypropylene composite material. The length-diameter ratio of the screws of the twin-screw extruder in this example was 40: 1.
The obtained pellets were injection molded into a standard test sample bar in an injection molding machine, and mechanical properties were measured using a universal tester and a pendulum impact tester, and the mechanical property data are shown in table 1.
TABLE 1 mechanical Properties of plant fiber reinforced Polypropylene composites
Note: the tensile test standard is GB/T1040-2006, and the tensile speed is 20 mm/min; the bending test standard is GB/T9341-2008 bending speed is 2 mm/min; the impact test standard is GB/T1843-2008.
As can be seen from Table 1, the tensile strength, flexural strength and impact strength of comparative example 1 are significantly lower than those of example 2, and the difference between the tensile strength, flexural strength and impact strength of comparative example 1 is that no compatibilizer is added in comparative example 1, dicumyl peroxide and diglycidyl itaconate are added in example 2, epoxy groups in the diglycidyl itaconate can perform coupling reaction with hydroxyl groups on the surface of plant fibers, and unsaturated double bonds contained in the diglycidyl itaconate perform grafting reaction with a polypropylene matrix to form covalent bonds under the action of radicals generated by dicumyl peroxide. Therefore, the itaconic acid diglycidyl ester plays a role of a bridge between the plant fiber and the polypropylene matrix, and the interface bonding force of the plant fiber and the polypropylene matrix is increased, so that the tensile strength and the bending strength are improved. In addition, after the itaconic acid diglycidyl ester which does not participate in the grafting reaction is coupled with the plant fiber, a layer of flexible interface phase is formed on the surface of the plant fiber, so that the energy generated by external force can be well absorbed, and the plant fiber reinforced polypropylene composite material has good impact strength.
It can also be seen from table 1 that the strength and modulus of comparative example 2 are significantly lower than example 2. Compared with the example 2, the organic peroxide is not added in the comparative example 2, only the epoxy group in the itaconic acid diglycidyl ester can perform coupling reaction with the hydroxyl on the surface of the plant fiber, the unsaturated double bond contained in the itaconic acid diglycidyl ester cannot perform grafting reaction with the polypropylene matrix to generate a covalent bond, the interfacial bonding force between the plant fiber and the polypropylene is improved to a limited extent, and the strength of the comparative example 2 is obviously lower than that of the example 2. In addition, the plasticizing effect of the diglycidyl itaconate in comparative example 2 is more remarkable, and the modulus thereof is lower than that of example 2.
Claims (8)
1. The plant fiber reinforced polypropylene composite material is characterized by being prepared from the following raw materials in parts by weight:
wherein the chemical structure of the itaconic acid diglycidyl ester is as formula I:
2. the plant fiber reinforced polypropylene composite material according to claim 1, which is prepared from the following raw materials in parts by weight:
3. the plant fiber reinforced polypropylene composite material according to claim 1, wherein the polypropylene is one or a combination of two of homo-polypropylene and a random copolymer of propylene and ethylene, and the melt index of the polypropylene is 5-50 g/10 min.
4. The plant fiber reinforced polypropylene composite material according to claim 1, wherein the plant fiber has a length of 3 to 40 mm.
5. The plant fiber reinforced polypropylene composite material of claim 1, wherein the organic peroxide is one or more of benzoyl peroxide, dicumyl peroxide, di-tert-butyl peroxide, lauroyl peroxide and 2-butanone peroxide.
6. The plant fiber reinforced polypropylene composite material of claim 1, wherein the lubricant is one or a mixture of more than two of polyethylene wax, polypropylene wax, polytetrafluoroethylene, butyl stearate, oleamide, erucamide or stearamide.
7. The plant fiber reinforced polypropylene composite material of claim 1, wherein the antioxidant is compounded by hindered phenol antioxidant and phosphite antioxidant according to the weight ratio of 1: 1.
8. A method for preparing the plant fiber reinforced polypropylene composite according to any one of claims 1 to 7, comprising:
uniformly mixing the polypropylene, the plant fiber, the organic peroxide, the itaconic acid diglycidyl ester, the lubricant and the antioxidant which are weighed according to the weight formula by using a high-speed mixer, and then carrying out melt blending extrusion, bracing, cooling and granulation by using a double-screw extruder to obtain plant fiber reinforced polypropylene composite material granules;
wherein the length-diameter ratio of the screws of the double-screw extruder is 30: 1-45: 1, and the melt blending temperature is 170-200 ℃.
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| CN114196115A (en) * | 2021-12-31 | 2022-03-18 | 天津金发新材料有限公司 | Polypropylene material and preparation method thereof |
| WO2023124710A1 (en) * | 2021-12-31 | 2023-07-06 | 天津金发新材料有限公司 | Polypropylene material and preparation method therefor |
| CN114196115B (en) * | 2021-12-31 | 2023-10-17 | 天津金发新材料有限公司 | Polypropylene material and preparation method thereof |
| CN114213760A (en) * | 2022-01-12 | 2022-03-22 | 安徽工程大学 | Hemp-coconut shell hybrid polypropylene composite material and preparation method and application thereof |
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