CN113789008A - Superstrong continuous fiber reinforced polyolefin composite material and preparation method thereof - Google Patents
Superstrong continuous fiber reinforced polyolefin 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
- 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
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
- C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials 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
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—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
- 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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- 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
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
Abstract
The invention discloses a superstrong continuous fiber reinforced polyolefin composite material and a preparation method thereof, wherein the material consists of polyolefin, glass fiber, compatilizer, glass powder, coupling agent, light stabilizer, antioxidant and lubricant; wherein the glass fibers are continuous fibers; the glass powder is boron glass powder with low melting point, and the grain diameter of the glass powder is 1-2 mu m. The preparation method of the material comprises the following steps: after the components of the polyolefin, the compatilizer, the light stabilizer, the antioxidant and the lubricant are premixed according to a certain proportion, the mixture is melted, mixed and extruded into an infiltration die through a double-screw extruder, the mixture and the specially treated continuous glass fiber are fully melted and infiltrated in the die, and the continuous production of the composite material is realized through a cooling and shaping device and a winding device for the fully impregnated continuous fiber reinforced polyolefin sheet. Due to the combination optimization of the interface of the fiber and the resin, the prepared composite material has ultrahigh mechanical strength.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a superstrong continuous fiber reinforced polyolefin composite material and a preparation method thereof.
Background
With the improvement of social development level and the enhancement of energy conservation, emission reduction, environmental protection and sustainable development consciousness, the fields of aerospace, rail transit, buildings, automobiles, household appliances and the like all put forward high-performance and light-weight requirements on materials. A single material has not been able to meet the practical needs of many areas and research has begun to turn the field of view gradually towards more prominent composite materials. Fiber reinforced resin based composite materials are developed in the united states from the last 30 th century, composite products at that time mainly meet the requirements of the military industry and the aerospace field, and are mainly classified into thermosetting types and thermoplastic types at present.
In the thermoplastic composite material type, compared with short fiber and long fiber reinforced thermoplastic composite materials, the continuous fiber reinforced thermoplastic composite material has more excellent mechanical properties and can be used as a structural material; in addition, the steel material has the advantages of light weight, corrosion resistance and the like, and has great potential. The tensile strength of Polyolefin (PO) is generally 20-30MPa, the tensile strength of long glass fiber reinforced polyolefin (LFTPO) is 150MPa, which is 3-5 times of that of pure resin, and the tensile strength of the conventional unidirectional continuous glass fiber reinforced sheet can reach 700-800MPa, although the strength is very high, the performance still needs to be further improved for application fields with very high requirements on weight, size and mechanics. At present, many researches on continuous fiber reinforced polyolefin composite materials are carried out, but most of the researches are focused on the development of some special functional materials and plates, such as low dielectric constant (CN106543554A), low odor (CN103374178A), flame retardation (CN102532681A), surface decoration (CN103963395A) and composite plates (CN103568396A and CN107877991A), and relatively few researches on the improvement of the tensile strength of the unidirectional tapes are carried out.
Disclosure of Invention
The invention aims to provide a superstrong continuous fiber reinforced polyolefin composite material and a preparation method thereof, compared with the existing continuous fiber reinforced polyolefin composite material, the superstrong continuous fiber reinforced polyolefin composite material has higher tensile strength, basically unchanged process and is suitable for batch continuous production.
The purpose of the invention can be realized by the following technical scheme:
an ultra-strong continuous fiber reinforced polyolefin composite material comprises the following components in parts by weight:
further, the polyolefin is one of polypropylene and polyethylene, the melt index of the polyolefin is 50-70g/10min, the test condition of the melt index of the polypropylene is 230 ℃, and the melt index of the polypropylene is 2.16 kg; the polyethylene melt index test condition is 190 ℃ and 2.16 kg.
Furthermore, the continuous glass fiber belongs to alkali-free glass fiber, and the alkali-free glass fiber has good electrical insulation and mechanical properties.
Further, the compatilizer is at least one of a cyclic anhydride grafted compatilizer and a carboxylic acid grafted compatilizer.
Furthermore, the light stabilizer is a benzotriazole light stabilizer, the benzotriazole light stabilizer can absorb ultraviolet rays with the wavelength of 270-380 nm, has good chemical stability, extremely small volatility and good compatibility with polyolefin, and is combined with an antioxidant to form a remarkable synergistic effect so as to improve the thermal oxygen stability of the product.
Further, the antioxidant is a compound antioxidant, and the compound antioxidant is prepared by mixing a phenol-resistant antioxidant: the volume ratio of the phosphite ester antioxidant is as follows: 1: (1.5-2) are compounded.
Furthermore, the lubricant is a fatty acid amide lubricant which has good chemical stability, high melting point, convenient processing, excellent external lubrication effect and stripping property, good transparency, dispersity, glossiness and electric insulation property, no toxicity and good compatibility with polyolefin.
A preparation method of a super-strong continuous fiber reinforced polyolefin composite material comprises the following steps:
s1, adding the polyolefin resin, the compatilizer, the light stabilizer, the antioxidant and the lubricant into a high-speed mixer at the temperature of 65-75 ℃ according to the proportion, and mixing for 5-10 min;
s2, the continuous glass fiber is guided by a yarn releasing and guide roller to enter a yarn spreading device for fiber strand dispersion, low-melting-point glass powder suspension is sprayed on the surface of the yarn spreading rear section, so that micron low-melting-point glass powder can be attached to the fiber strand while the fiber strand is dispersed, and then the fiber strand is guided by the guide roller to continuously enter a high-temperature furnace for baking for 5-10S, wherein the temperature of the high-temperature furnace is as follows: 400-450 ℃, and then the mixture is guided into a dipping die through another guide roller;
s3, adding the material in the S1 into a main feeding port of a double-screw extruder under the protection of nitrogen, melting, mixing and extruding the material into an impregnation die through the double-screw extruder, shunting, melting and impregnating the material with the continuous fiber treated in the S2, cooling and shaping the fully impregnated continuous fiber bundle through a cooling and shaping device, and carrying out continuous production under the drive of a traction and winding device, wherein the temperature of the double-screw extruder is 220-.
Further, the low-melting-point glass powder is subjected to high-speed stirring and dispersing treatment by using a coupling agent, the mass ratio of the coupling agent to the low-melting-point glass powder is 0.002-0.0025, and the stirring rotating speed is as follows: 1000-1200r/min for 40-50min, adding the surface-treated micron low-melting-point glass powder into water to prepare a solution with the micron low-melting-point glass powder accounting for 1-1.5%, performing ultrasonic treatment for 1-1.5h at the ultrasonic frequency of 28kHz or 40kHz to obtain a low-melting-point glass powder suspension, performing high-speed stirring and dispersing treatment to remove the agglomeration among the particles of the low-melting-point glass powder, and uniformly dispersing the particles on the surface of the glass fiber in the spraying process.
Further, the coupling agent is at least one of 3-aminopropyltriethoxysilane or 3-glycidoxypropyltrimethoxysilane; the grain diameter of the micron low-melting-point glass powder is 1-2 mu m, and the melting point is 350-400 ℃.
The invention has the beneficial effects that:
1. after the spreading continuous glass fiber is sprayed with the low-melting-point glass powder turbid liquid and is heated, the micron glass micropowder is slightly melted and adhered to the surface of the smooth glass fiber to form the surface of the glass fiber with certain roughness, and the rough surface can form a strong mechanical occlusion effect at the interface of the fiber and the resin, so that the tensile strength of the unidirectional tape can be greatly increased;
2. the organic-inorganic interface action of the active group compatilizer in the composite material is enhanced; the compatilizer added into the resin can increase active reaction groups in the resin matrix, so that the resin matrix can be effectively combined with inorganic micron glass micro powder and continuous glass fibers, the bonding force of an interface is enhanced, and the tensile strength of the unidirectional tape is improved.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a super-strong continuous fiber reinforced polyolefin composite material comprises the following steps:
s1, adding 35 kg of polypropylene resin, 4 kg of cyclic anhydride grafted compatilizer, 0.2 kg of benzotriazole light stabilizer, 0.2 kg of compound antioxidant and 0.2 kg of lubricant into a high-speed mixer at the temperature of 65 ℃ for mixing for 5min, wherein the compound antioxidant is prepared by mixing the following components in parts by weight: the volume ratio of the phosphite ester antioxidant is as follows: 1: 1.5; the lubricant is a fatty acid amide lubricant.
S2, carrying out high-speed stirring and dispersing treatment on the micron low-melting-point glass powder by using a coupling agent, wherein the mass ratio is as follows: the coupling agent/low-melting glass powder is 0.002, and the stirring speed is as follows: 1200r/min for 40min, then adding the surface-treated micron low-melting-point glass powder into water to prepare a solution with the micron low-melting-point glass powder accounting for 1%, then carrying out ultrasonic treatment for 1h at the ultrasonic frequency of 28kHz to obtain a low-melting-point glass powder suspension, carrying out high-speed stirring and dispersing treatment to remove agglomeration among particles of the low-melting-point glass powder, and uniformly dispersing the particles on the surface of glass fibers in a spraying process, wherein the particle size of the micron low-melting-point glass powder is 1-2 mu m and the particle size of the micron low-melting-point glass powder is 1-2 mu m.
The coupling agent is 3-aminopropyl triethoxysilane.
S3, 59 kg of continuous glass fiber enters a yarn spreading device for fiber bundle dispersion through yarn releasing and guide rollers, 2 kg of low-melting-point glass powder suspension is sprayed on the surface of the rear yarn spreading section, so that micron low-melting-point glass powder can be attached to fiber bundles while the fiber bundles are dispersed, and then the fiber bundles are guided by the guide rollers to continuously enter a high-temperature furnace for baking for 5S (the micron low-melting-point glass micropowder is slightly melted and adhered to the surface of the smooth glass fiber, and excessive water is evaporated with the micron low-melting-point glass micropowder), wherein the temperature of the high-temperature furnace is 400 ℃, and then the fiber bundles are guided by another guide roller to enter a dipping die;
and S4, adding the material in the S1 into a main feeding port of a double-screw extruder under the protection of nitrogen, melting, mixing and extruding the material into an impregnation die through the double-screw extruder, shunting, melting and impregnating the material with the continuous fiber treated in the S3, cooling and shaping the fully impregnated continuous fiber bundle through a cooling and shaping device, and carrying out continuous production under the driving of a traction and winding device. In the processing process, the temperature of the double-screw extruder is 220 ℃, the rotating speed of the screw is 450RPM, the vacuum degree is-0.04 MPa, and the temperature of the dipping die is 230 ℃.
Comparative example 1
The difference from example 1 is that: does not contain a low-melting-point glass powder suspension.
Comparative example 2
The difference from example 1 is that: the temperature of the high-temperature furnace in S3 was 100 ℃.
Comparative example 3
The difference from example 1 is that: in S2, a coupling agent is used to carry out high-speed stirring and dispersion treatment on the micron glass powder with the melting point of 480-520 ℃.
Example 2
A preparation method of a super-strong continuous fiber reinforced polyolefin composite material comprises the following steps:
s1, adding 37 kg of polyethylene resin, 5 kg of carboxylic acid graft type compatilizer, 0.3 kg of benzotriazole light stabilizer, 0.3 kg of compound antioxidant and 0.3 kg of lubricant into a high-speed mixer at the temperature of 75 ℃ for mixing for 10min, wherein the compound antioxidant is prepared by mixing the following components in percentage by weight: the volume ratio of the phosphite ester antioxidant is as follows: 1: 2; the lubricant is a fatty acid amide lubricant.
S2, carrying out high-speed stirring and dispersing treatment on the micron low-melting-point glass powder by using a coupling agent, wherein the mass ratio is as follows: the coupling agent/low-melting-point glass powder is 0.0025, and the stirring speed is as follows: 1000r/min for 50min, adding the surface-treated micron low-melting-point glass powder into water to prepare a solution with the micron low-melting-point glass powder accounting for 1.5%, performing ultrasonic treatment for 1.5h at the ultrasonic frequency of 40kHz to obtain a low-melting-point glass powder suspension, performing high-speed stirring and dispersing treatment to remove the agglomeration among the particles of the low-melting-point glass powder, uniformly dispersing the low-melting-point glass powder on the surface of glass fibers in a spraying process, wherein the particle size of the micron low-melting-point glass powder is 1-2 mu m, and the melting point is 350-400 ℃.
The coupling agent is 3-glycidyl ether oxypropyl trimethoxy silane.
S3, leading 61 kg of continuous glass fiber to enter a yarn spreading device for fiber strand dispersion through yarn releasing and a guide roller, spraying 3 kg of low-melting-point glass powder suspension on the surface of the yarn spreading rear section to ensure that micron low-melting-point glass powder can be attached to fiber bundles while the fiber bundles are dispersed, then leading the fiber bundles to continuously enter a high-temperature furnace through the guide roller to be baked for 10S (the micron low-melting-point glass micro powder is slightly melted and adhered to the surface of smooth glass fiber, and excessive water is evaporated along with the micron low-melting-point glass micro powder), controlling the temperature of the high-temperature furnace to be 450 ℃, and then leading the fiber bundles to enter a dipping die through another guide roller;
s4: under the protection of nitrogen, adding the material in the S1 into a main feeding port of a double-screw extruder, melting, mixing and extruding the material into an impregnation die through the double-screw extruder, shunting, melting and impregnating the material with the continuous fiber treated in the S3, cooling and shaping the fully impregnated continuous fiber bundle through a cooling and shaping device, and carrying out continuous production under the driving of a traction and winding device. In the processing process, the temperature of the double-screw extruder is 235 ℃, the rotating speed of the screw is 500RPM, the vacuum degree is-0.1 MPa, and the temperature of the dipping die is 240 ℃.
Comparative example 4
The difference from example 2 is that: does not contain a low-melting-point glass powder suspension.
The polyolefin melt index is 50-70g/10min, and the polypropylene melt index test condition is 230 ℃ and 2.16 kg; the polyethylene melt index test condition is 190 ℃ and 2.16 kg.
The continuous glass fiber is alkali-free glass fiber.
Comparative example 5
The difference from example 2 is that: no compatibilizing agent is included.
The composite materials obtained in comparative examples 1 to 3, example 1 and example 2 were subjected to tensile strength tests, and the test results are shown in the following table; the composites obtained in examples 1 and 2 exhibit ultra high tensile strength. Example 1 tensile strength is higher than comparative example 1, which shows that the tensile strength of the low-melting glass micropowder to the continuous fiber is obviously improved; the tensile strength of the comparative example 2 is not much different from that of the comparative example 3, and is larger than that of the comparative example 1, but the tensile strength of the comparative example 1 is far lower than that of the comparative example 1, which shows that in the case of fusion bonding of the low-melting-point glass micropowder, although weak coupling effect exists between the glass micropowder and the continuous glass fiber, the strong bonding effect is far smaller than that of the fusion bonding, so that the high tensile strength in the example 1 is derived from the fusion bonding effect of the low-melting-point glass micropowder and the continuous glass fiber. The tensile strength of the comparative example 5 is far lower than that of the example 2, which shows that the compatibility between the organic resin matrix and the inorganic micron glass micro powder and the continuous glass fiber is poor, the tensile strength is low, and the organic-inorganic interface compatibilization effect of the compatilizer is very important for improving the tensile strength.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (10)
1. The super-strong continuous fiber reinforced polyolefin composite material is characterized by comprising the following components in parts by weight:
stirring and dispersing the low-melting-point glass powder by using a coupling agent, wherein the mass ratio of the coupling agent to the low-melting-point glass powder is 0.002-0.0025, adding the micrometer low-melting-point glass powder subjected to surface treatment into water to prepare a solution with the micrometer low-melting-point glass powder accounting for 1-1.5%, and then carrying out ultrasonic treatment to obtain a low-melting-point glass powder suspension.
2. The ultra-strong continuous fiber reinforced polyolefin composite material as claimed in claim 1, wherein the polyolefin is one of polypropylene and polyethylene, the melt index of the polyolefin is 50-70g/10min, the polypropylene melt index test condition is 230 ℃, 2.16 kg; the polyethylene melt index test condition is 190 ℃ and 2.16 kg.
3. The ultra-strong continuous fiber reinforced polyolefin composite material of claim 1, wherein the continuous glass fiber is an alkali-free glass fiber.
4. The super-strong continuous fiber reinforced polyolefin composite material according to claim 1, wherein the compatibilizer is at least one of a cyclic anhydride grafted compatibilizer and a carboxylic acid grafted compatibilizer.
5. The ultra-strong continuous fiber reinforced polyolefin composite material as claimed in claim 1, wherein the light stabilizer is a benzotriazole light stabilizer.
6. The ultra-strong continuous fiber reinforced polyolefin composite material according to claim 1, wherein the antioxidant is a compound antioxidant, and the compound antioxidant is prepared by mixing a phenol-hindered antioxidant: the volume ratio of the phosphite ester antioxidant is as follows: 1: (1.5-2) are compounded.
7. The super strong continuous fiber reinforced polyolefin composite of claim 1, wherein said lubricant is a fatty acid amide lubricant.
8. The method for preparing a composite material according to any one of claims 1 to 7, characterized in that it comprises the following steps:
s1, adding the polyolefin resin, the compatilizer, the light stabilizer, the antioxidant and the lubricant into a high-speed mixer together according to the proportion, and mixing for 5-10min at 65-75 ℃;
s2, the continuous glass fiber enters the yarn spreading device for fiber strand dispersion through yarn releasing and guide roller guiding, low-melting-point glass powder suspension is sprayed on the surface of the yarn spreading rear section, so that micron low-melting-point glass powder is attached to the fiber strand while the fiber strand is dispersed, and then the fiber strand continuously enters the high-temperature furnace for baking for 5-10S through guide roller guiding, wherein the temperature of the high-temperature furnace is as follows: 400-450 ℃, and then the mixture is guided into a dipping die through another guide roller;
s3, adding the material in the S1 into a main feeding port of a double-screw extruder under the protection of nitrogen, melting, mixing and extruding the material into an impregnation die through the double-screw extruder, shunting, melting and impregnating the material with the continuous fiber treated in the S2, cooling and shaping the fully impregnated continuous fiber bundle through a cooling and shaping device, and carrying out continuous production under the drive of a traction and winding device, wherein the temperature of the double-screw extruder is 220-.
9. The method for preparing the composite material according to claim 8, wherein the stirring speed of the low-melting-point glass powder is as follows during stirring and dispersing treatment by using the coupling agent: 1000-1200r/min for 40-50min, ultrasonic time for 1-1.5h and ultrasonic frequency of 28kHz or 40kHz, and the stirring and dispersing treatment removes the agglomeration among the low-melting-point glass powder particles and can uniformly disperse on the surface of the glass fiber in the spraying process.
10. The method of claim 9, wherein the coupling agent is at least one of 3-aminopropyltriethoxysilane or 3-glycidoxypropyltrimethoxysilane; the grain diameter of the micron low-melting-point glass powder is 1-2 mu m, and the melting point is 350-400 ℃.
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Cited By (1)
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| WO2023201778A1 (en) * | 2022-04-21 | 2023-10-26 | 上迈(镇江)新能源科技有限公司 | Photovoltaic module composite backboard and preparation method therefor, and photovoltaic module |
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| CN113789008B (en) | 2022-12-13 |
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