CN116178846B - Anti-fatigue PP alloy material and preparation method thereof - Google Patents
Anti-fatigue PP alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of high polymer materials, and particularly relates to an anti-fatigue PP alloy material and a preparation method thereof. The product comprises polypropylene fibers and nylon 6 fibers; wherein the polypropylene fiber comprises: fine and coarse fibers; the length-diameter ratio of the fine fiber is 500-600; the length-diameter ratio of the crude fiber is 30-60; the length-diameter ratio of the nylon 6 fiber is 250-320; the mass ratio of the fine fiber to the coarse fiber is 1:2-2.5; the mass ratio of the polypropylene fiber to the nylon 6 fiber is 3:1 to 1.5; maleic anhydride is grafted on the surface of the crude fiber, and the crude fiber is fixedly connected with the nano graphene oxide through the maleic anhydride. Wherein, nonionic surfactant is embedded between the layers of the nano graphene oxide; and the particle size distribution range of the nano graphene oxide is 10-30nm.
Description
Technical Field
The invention belongs to the technical field of high polymer materials. More particularly, relates to an anti-fatigue PP alloy material and a preparation method thereof.
Background
The polypropylene (PP) resin has the advantages of good processability, good chemical resistance, good water absorption resistance and the like, but at the same time has the defects of low notch impact strength, poor heat resistance, poor dimensional stability and the like under normal temperature conditions, so that the PP resin is easy to damage when being subjected to stress circulation under the condition of alternating load in the working condition using process. .
Nylon (PA) is one of important engineering plastics, which has excellent mechanical properties, heat resistance, abrasion resistance and high hardness, but is a difficult problem in processing and application because it easily absorbs water to cause degradation of product properties.
The alloy material is prepared by utilizing two materials, namely PP and PA, and the two materials are blended so as to realize mutual modification, thereby taking advantage of the advantages and the disadvantages. However, PP belongs to a nonpolar polymer, PA belongs to a polar polymer, the polarity difference of the PP and the PA is very large, and the alloy performance obtained by direct blending is poor; in particular, due to the compatibility of the alloy material and the alloy material, the alloy material is also easy to break when being subjected to bending stress under the condition of alternating load. Therefore, how to fully utilize the improvement of the overall performance of the PP and the PA after being combined in the blending modification process, and simultaneously, the improvement of the bending resistance of the product and the extension of the service life of the product are considered, and are one of technical problems facing the technicians in the field.
Disclosure of Invention
The invention aims to overcome the defects that when the existing PP alloy material is compounded by adopting PP and PA, the alloy material is easily damaged and insufficient when being subjected to bending stress under the condition of alternating load after the two materials are comprehensively compounded due to the large difference of polarities of the PP and PA, and provides an anti-fatigue PP alloy material and a preparation method thereof.
The invention aims to provide an anti-fatigue PP alloy material.
The invention further aims to provide a preparation method of the anti-fatigue PP alloy material.
The above object of the present invention is achieved by the following technical scheme:
an anti-fatigue PP alloy material comprises polypropylene fibers and nylon 6 fibers;
wherein the polypropylene fiber comprises: fine and coarse fibers;
the length-diameter ratio of the fine fiber is 500-600;
the length-diameter ratio of the crude fiber is 30-60;
the length-diameter ratio of the nylon 6 fiber is 250-320;
the mass ratio of the fine fiber to the coarse fiber is 1:2-2.5;
the mass ratio of the polypropylene fiber to the nylon 6 fiber is 3:1 to 1.5;
maleic anhydride is grafted on the surface of the crude fiber, and the crude fiber is fixedly connected with the nano graphene oxide through the maleic anhydride.
Firstly, in the technical scheme, the coarse polypropylene fiber is taken as one of matrix fibers, and maleic anhydride is grafted on the surface of the matrix fiber, so that nano-sized graphene oxide is captured and adsorbed and fixed, and the roughness of the original smooth coarse fiber surface is effectively improved; according to the method, polypropylene fine fibers and nylon 6 fibers with a certain length-diameter ratio are added, so that the polypropylene fine fibers and the nylon 6 fibers which are more slender than the coarse fibers can be entangled on the surfaces of the coarse fibers, and the maleic anhydride has good compatibility to the coarse fibers, the fine fibers and the nylon 6 fibers, so that the fine fibers and the nylon 6 fibers have certain looseness in entanglement on the surfaces of the coarse fibers, and after the nano graphene oxide is fixed, due to the fact that the graphene oxide is in a lamellar structure, the occurrence of the lamellar structure of the nano graphene oxide can be effectively avoided, and the entanglement and the loose of the entangled points of the fine fiber nylon 6 fibers on the surfaces of the coarse fibers can be effectively avoided when the external force acts on the fine fiber nylon 6 fibers; based on the construction of the complex three-dimensional network structure, the alloy material system after compounding has certain flexibility, and under the condition of alternating load, the alloy material can release stress by using the three-dimensional network structure freely when bearing stress circulation, and permanent deformation or fracture is avoided, so that the fatigue resistance of the product is effectively improved.
Further, a surfactant is embedded between the layers of the nano graphene oxide.
Further, the surfactant is a nonionic surfactant; the nonionic surfactant is selected from the group consisting of: any one of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyoxyethylene sorbitan ester and coconut oil fatty acid diacetyl amide.
According to the technical scheme, the surfactant is further introduced between the layers of the nano graphene oxide, so that the interlayer spacing of the graphene oxide can be effectively widened, the graphene oxide is used as a binding site, and the graphene oxide can be contracted and expanded at a certain interlayer spacing in the stress circulation process, so that the effect of releasing stress is achieved.
Further, the particle size distribution range of the nano graphene oxide is 10-30nm.
According to the technical scheme, the nano graphene oxide with a narrow particle size distribution range is further selected as the raw material, so that the properties of the graphene oxide adsorbed by different points tend to be more consistent, the performance difference between different points in the alloy material is reduced as much as possible, and local failure is avoided.
Further, the length-diameter ratio of the nylon 6 fiber is 1/2 of the length-diameter ratio of the fine fiber; and the aspect ratio of the coarse fibers is 8% of the aspect ratio of the fine fibers.
According to the technical scheme, nylon 6 fibers, fine fibers and coarse fibers with specific length-diameter ratios are further selected, so that when different fibers and fibers are intertwined, the fine fibers and the coarse fibers have enough different flexibilities, so that the fine fibers are more easily entangled and fixed on the surface of the coarse fibers, and the coarse fibers can play a better supporting role by virtue of the effects of maleic anhydride and graphene.
Further, the diameter of the coarse fiber is 450-500 μm, the diameter of the fine fiber is 20-30 μm, and the diameter of the nylon 6 fiber is 30-40 μm.
The preparation method of the anti-fatigue PP alloy material comprises the following specific preparation steps:
weighing the components according to the composition of the raw materials;
carrying out grafting modification on the surface of the crude fiber by adopting maleic anhydride to obtain crude fiber grafted with maleic anhydride;
dispersing the crude fiber grafted with maleic anhydride in absolute ethyl alcohol, adding nano graphene oxide into the absolute ethyl alcohol, stirring for reaction at 50-55 ℃ after uniform ultrasonic dispersion, and carrying out suction filtration, washing and drying to remove residual ethanol and obtain crude fiber adsorbed with graphene oxide;
and uniformly mixing the coarse fibers, the fine fibers and the nylon 6 fibers adsorbed with the graphene oxide, extruding the mixture through a double-screw extruder, and carrying out traction, drying and granulating, and then carrying out injection molding to obtain the product.
Further, the specific preparation steps further include:
preprocessing the graphene oxide; the pretreatment comprises the following steps: dispersing graphene oxide in water, adding a surfactant with the mass of 10-12% of that of the graphene oxide, performing ultrasonic dispersion, heating and stirring to react, standing at room temperature for 8-12h, and performing suction filtration, washing and drying to complete pretreatment.
Further, when maleic anhydride is adopted to carry out grafting modification on the surface of the crude fiber, firstly, the crude fiber is washed and dried by acetone, then is mixed with a dimethylbenzene mixed solution of maleic anhydride and benzophenone, then is subjected to ultraviolet light-induced reaction, and then is filtered, washed and dried to obtain the crude fiber grafted with the maleic anhydride.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Reagents and materials used in the following examples are commercially available unless otherwise specified.
Example 1
Pretreatment of graphene oxide:
the nano graphene oxide and deionized water are mixed according to the mass ratio of 1:8, after mixing, stirring and dispersing for 20min at 600r/min by using a stirrer, adding a surfactant with 10% of the mass of the nano graphene oxide, then performing ultrasonic dispersion for 2h at an ultrasonic frequency of 80kHz, heating and stirring for reacting for 2h at a temperature of 50 ℃ and a stirring speed of 400r/min, standing for 8h at room temperature, performing suction filtration, collecting a filter cake, washing the filter cake with deionized water for 4 times, transferring the washed filter cake into an oven, and drying to constant weight at a temperature of 85 ℃ to obtain pretreated graphene oxide; the particle size distribution range of the nano graphene oxide is 10-30nm; the surfactant is a nonionic surfactant; the nonionic surfactant is selected from the group consisting of: polyoxyethylene sorbitan esters;
crude fiber grafted maleic anhydride:
soaking the crude fiber in acetone for 20 hours, taking out, and drying in a 60 ℃ oven to obtain pretreated crude fiber; and then the mass ratio is 5:1:20, mixing the pretreated crude fiber, maleic anhydride and a dimethylbenzene mixed solution of benzophenone with the mass fraction of 10%, transferring the mixture into an ultraviolet lamp box, irradiating the mixture with ultraviolet light for 0.5h, filtering the mixture, washing the obtained filter cake with acetone for 2 times, and drying the filter cake in a baking oven at 60 ℃ to constant weight to obtain crude fiber grafted with maleic anhydride;
adsorption fixing pretreatment graphene oxide:
sequentially taking 40 parts of crude fibers grafted with maleic anhydride, 120 parts of absolute ethyl alcohol and 6 parts of pretreated graphene oxide according to parts by weight, firstly mixing the crude fibers grafted with maleic anhydride and the absolute ethyl alcohol, then adding the pretreated graphene oxide, performing ultrasonic dispersion for 10min under the condition of ultrasonic frequency of 80kHz, then stirring and reacting for 45min under the condition of 50 ℃, performing suction filtration, collecting a filter cake, washing the filter cake with the absolute ethyl alcohol for 2 times, and drying to remove residual ethanol, thereby obtaining crude fibers adsorbed with the graphene oxide;
preparation of alloy materials:
uniformly mixing coarse fibers, fine fibers and nylon 6 fibers adsorbed with graphene oxide, extruding the mixture through a double-screw extruder, drawing, drying and cutting the mixture into particles with the particle size of 12mm, and performing injection molding, wherein the injection molding temperature is 230 ℃, thus obtaining a product;
wherein the fine fiber has an aspect ratio of 500; the fine fibers are polypropylene fine fibers;
the length-diameter ratio of the crude fiber adsorbed with graphene oxide is 30; the crude fiber is polypropylene crude fiber;
the length-diameter ratio of the nylon 6 fiber is 250;
specifically, the diameter of the fine fiber is 20 mu m, the diameter of the coarse fiber is 450 mu m, and the diameter of the nylon 6 fiber is 30 mu m;
the mass ratio of the fine fibers to the coarse fibers adsorbed with graphene oxide is 1:2;
the total mass of the fine fibers and the coarse fibers adsorbed with the graphene oxide is the total mass of polypropylene fibers, and the mass ratio of the polypropylene fibers to the nylon 6 fibers is 3:1.
example 2
Pretreatment of graphene oxide:
the nano graphene oxide and deionized water are mixed according to the mass ratio of 1:10, stirring and dispersing for 30min at a rotating speed of 700r/min by using a stirrer, adding a surfactant with 11% of the mass of the nano graphene oxide, performing ultrasonic dispersion for 3h at an ultrasonic frequency of 90kHz, heating and stirring for reacting for 3h at a temperature of 52 ℃ and a stirring rotating speed of 500r/min, standing for 10h at room temperature, performing suction filtration, collecting a filter cake, washing the filter cake with deionized water for 5 times, transferring the washed filter cake into an oven, and drying to constant weight at a temperature of 90 ℃ to obtain pretreated graphene oxide; the particle size distribution range of the nano graphene oxide is 10-30nm; the surfactant is a nonionic surfactant; the nonionic surfactant is selected from the group consisting of: alkylphenol ethoxylates;
crude fiber grafted maleic anhydride:
soaking the crude fiber in acetone for 22 hours, taking out, and drying in a 62 ℃ oven to obtain pretreated crude fiber; and then the mass ratio is 5:1:20, mixing the pretreated crude fiber, maleic anhydride and a dimethylbenzene mixed solution of benzophenone with the mass fraction of 10%, transferring the mixture into an ultraviolet lamp box, irradiating the mixture with ultraviolet light for 0.8h, filtering the mixture, washing the obtained filter cake with acetone for 3 times, and drying the filter cake in an oven at 62 ℃ to constant weight to obtain crude fiber grafted with maleic anhydride;
adsorption fixing pretreatment graphene oxide:
sequentially taking 45 parts of crude fibers grafted with maleic anhydride, 130 parts of absolute ethyl alcohol and 7 parts of pretreated graphene oxide according to parts by weight, firstly mixing the crude fibers grafted with maleic anhydride and the absolute ethyl alcohol, then adding the pretreated graphene oxide, performing ultrasonic dispersion for 15min under the condition of ultrasonic frequency of 90kHz, then stirring and reacting for 50min under the condition of 52 ℃, performing suction filtration, collecting a filter cake, washing the filter cake with the absolute ethyl alcohol for 3 times, and drying to remove residual ethanol, thereby obtaining crude fibers adsorbed with the graphene oxide;
preparation of alloy materials:
uniformly mixing coarse fibers, fine fibers and nylon 6 fibers adsorbed with graphene oxide, extruding the mixture through a double-screw extruder, drawing, drying and cutting the mixture into particles with the particle size of 11mm, and performing injection molding at the injection temperature of 235 ℃ to obtain a product;
wherein the fine fiber has an aspect ratio of 550; the fine fibers are polypropylene fine fibers;
the length-diameter ratio of the crude fiber adsorbed with the graphene oxide is 40; the crude fiber is polypropylene crude fiber;
specifically, the diameter of the fine fiber is 25 μm, the diameter of the coarse fiber is 480 μm, and the diameter of the nylon 6 fiber is 35 μm;
the length-diameter ratio of the nylon 6 fiber is 300;
the mass ratio of the fine fibers to the coarse fibers adsorbed with graphene oxide is 1:2.2;
the total mass of the fine fibers and the coarse fibers adsorbed with the graphene oxide is the total mass of polypropylene fibers, and the mass ratio of the polypropylene fibers to the nylon 6 fibers is 3:1.2.
example 3
Pretreatment of graphene oxide:
the nano graphene oxide and deionized water are mixed according to the mass ratio of 1:12, stirring and dispersing for 40min at a rotating speed of 800r/min by using a stirrer, adding a surfactant with the mass of 12% of the nano graphene oxide, performing ultrasonic dispersion for 4h at an ultrasonic frequency of 100kHz, heating and stirring for reacting for 4h at a temperature of 55 ℃ and a stirring rotating speed of 600r/min, standing for 12h at room temperature, performing suction filtration, collecting a filter cake, washing the filter cake with deionized water for 6 times, transferring the washed filter cake into an oven, and drying to constant weight at a temperature of 95 ℃ to obtain pretreated graphene oxide; the particle size distribution range of the nano graphene oxide is 10-30nm; the surfactant is a nonionic surfactant; the nonionic surfactant is selected from the group consisting of: fatty alcohol polyoxyethylene ether;
crude fiber grafted maleic anhydride:
soaking the crude fiber in acetone for 24 hours, taking out, and drying in a 65 ℃ oven to obtain pretreated crude fiber; and then the mass ratio is 5:1:20, mixing the pretreated crude fiber, maleic anhydride and a dimethylbenzene mixed solution of benzophenone with the mass fraction of 10%, transferring into an ultraviolet lamp box, irradiating with ultraviolet light for 1h, filtering, washing the obtained filter cake with acetone for 4 times, and drying in a drying oven at 65 ℃ to constant weight to obtain crude fiber grafted with maleic anhydride;
adsorption fixing pretreatment graphene oxide:
sequentially taking 50 parts of crude fibers grafted with maleic anhydride, 150 parts of absolute ethyl alcohol and 8 parts of pretreated graphene oxide according to parts by weight, firstly mixing the crude fibers grafted with maleic anhydride and the absolute ethyl alcohol, then adding the pretreated graphene oxide, performing ultrasonic dispersion for 20min under the condition of ultrasonic frequency of 100kHz, then stirring and reacting for 60min under the condition of temperature of 55 ℃, performing suction filtration, collecting a filter cake, washing the filter cake with the absolute ethyl alcohol for 4 times, and drying to remove residual ethanol, thereby obtaining crude fibers adsorbed with the graphene oxide;
preparation of alloy materials:
uniformly mixing coarse fibers, fine fibers and nylon 6 fibers adsorbed with graphene oxide, extruding the mixture through a double-screw extruder, drawing, drying and cutting the mixture into particles with the particle size of 12mm, and performing injection molding, wherein the injection molding temperature is 240 ℃, thus obtaining a product;
wherein the fine fiber has an aspect ratio of 600; the fine fibers are polypropylene fine fibers;
the length-diameter ratio of the crude fiber adsorbed with graphene oxide is 60; the crude fiber is polypropylene crude fiber;
the length-diameter ratio of the nylon 6 fiber is 320;
specifically, the diameter of the fine fiber is 30 mu m, the diameter of the coarse fiber is 500 mu m, and the diameter of the nylon 6 fiber is 40 mu m;
the mass ratio of the fine fibers to the coarse fibers adsorbed with graphene oxide is 1:2.5;
the total mass of the fine fibers and the coarse fibers adsorbed with the graphene oxide is the total mass of polypropylene fibers, and the mass ratio of the polypropylene fibers to the nylon 6 fibers is 3:1.5.
example 4
The difference between this embodiment and embodiment 1 is that: in the pretreatment process of graphene oxide, a nonionic surfactant is not added, and the rest conditions are kept unchanged.
Example 5
The difference between this embodiment and embodiment 1 is that: and replacing the graphene oxide with the particle size distribution range of 10-30nm by adopting the graphene oxide with the particle size distribution range of 10-100nm with equal mass, and keeping the rest conditions unchanged.
Example 6
The difference between this embodiment and embodiment 1 is that: and replacing the graphene oxide with the particle size distribution range of 10-30nm by adopting the graphene oxide with the particle size distribution range of 40-60nm with equal mass, and keeping the rest conditions unchanged.
Example 7
The difference between this embodiment and embodiment 1 is that: the fine fiber has an aspect ratio of 500; the length-diameter ratio of the nylon 6 fiber is 250; the aspect ratio of the crude fiber is 40;
specifically, the diameter of the fine fiber is 20 μm, the diameter of the coarse fiber is 450 μm, and the diameter of the nylon 6 fiber is 30 μm.
Comparative example 1
This comparative example is different from example 1 in that: after the crude fiber is grafted with maleic anhydride, pretreated graphene oxide is not added, so that the pretreated graphene oxide is not adsorbed and fixed on the surface of the crude fiber in the product, and the rest conditions are kept unchanged.
Comparative example 2
This comparative example is different from example 1 in that: the crude fibers were not grafted with maleic anhydride and the remaining conditions remained unchanged.
Comparative example 3
This comparative example is different from example 1 in that: and adopting polypropylene fine fibers with the equal mass diameter of 20 mu m and the length-diameter ratio of 500 to replace coarse fibers to graft maleic anhydride, and carrying out subsequent treatment of adsorbing and fixing pretreatment graphene oxide, wherein the rest conditions are kept unchanged.
Comparative example 4
This comparative example is different from example 1 in that: the glass fiber with equal quality is adopted to replace the crude fiber adsorbed with the graphene oxide, and the rest conditions are kept unchanged.
The products obtained in examples 1 to 7 and comparative examples 1 to 4 were subjected to performance tests, and specific test methods and test results are as follows:
the products of each example or comparative example with the dimensions of 120mm multiplied by 3mm are selected as test samples, and the bending performance of the products is tested according to ISO 178-2010, wherein the bending speed is 2mm/min, and the bending strength and the bending elastic modulus of the products are obtained;
table 1: product performance test results
As shown by the test results in Table 1, the product obtained by the invention can effectively resist bending stress and has good mechanical properties.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (7)
1. An anti-fatigue PP alloy material is characterized by comprising polypropylene fibers and nylon 6 fibers;
wherein the polypropylene fiber comprises: fine and coarse fibers;
the length-diameter ratio of the fine fiber is 500-600;
the length-diameter ratio of the crude fiber is 30-60;
the length-diameter ratio of the nylon 6 fiber is 250-320;
the mass ratio of the fine fiber to the coarse fiber is 1:2-2.5, wherein the diameter of the coarse fiber is 450-500 mu m, the diameter of the fine fiber is 20-30 mu m, and the diameter of the nylon 6 fiber is 30-40 mu m;
the mass ratio of the polypropylene fiber to the nylon 6 fiber is 3:1 to 1.5;
maleic anhydride is grafted on the surface of the crude fiber, and the crude fiber is fixedly connected with nano graphene oxide through the maleic anhydride;
the anti-fatigue PP alloy material is prepared by the following steps:
carrying out grafting modification on the surface of the crude fiber by adopting maleic anhydride to obtain crude fiber grafted with maleic anhydride;
dispersing the crude fiber grafted with maleic anhydride in absolute ethyl alcohol, adding nano graphene oxide into the absolute ethyl alcohol, stirring for reaction at 50-55 ℃ after uniform ultrasonic dispersion, and carrying out suction filtration, washing and drying to remove residual ethanol and obtain crude fiber adsorbed with graphene oxide;
and uniformly mixing the coarse fibers, the fine fibers and the nylon 6 fibers adsorbed with the graphene oxide, extruding the mixture through a double-screw extruder, and carrying out traction, drying and granulating, and then carrying out injection molding to obtain the product.
2. The anti-fatigue PP alloy material of claim 1, wherein a surfactant is embedded between the layers of the nano graphene oxide.
3. The anti-fatigue PP alloy material of claim 2, wherein the surfactant is a nonionic surfactant; the nonionic surfactant is selected from the group consisting of: any one of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyoxyethylene sorbitan ester and coconut oil fatty acid diacetyl amide.
4. An anti-fatigue PP alloy material according to any of claims 1-3, wherein the nano graphene oxide has a particle size distribution in the range of 10-30nm.
5. The anti-fatigue PP alloy material of claim 1, wherein the nylon 6 fiber has an aspect ratio of 1/2 of the aspect ratio of the fine fiber; and the aspect ratio of the coarse fibers is 8% of the aspect ratio of the fine fibers.
6. The anti-fatigue PP alloy material of claim 1, wherein the preparing step further comprises:
preprocessing the nano graphene oxide; the pretreatment comprises the following steps: dispersing nano graphene oxide in water, adding surfactant with the mass of 10-12% of the nano graphene oxide, performing ultrasonic dispersion, heating and stirring for reaction, standing at room temperature for 8-12h, and performing suction filtration, washing and drying to complete pretreatment.
7. The anti-fatigue PP alloy material of claim 1, wherein the method for grafting modification of the surface of the crude fiber with maleic anhydride comprises:
washing and drying crude fiber with acetone, mixing with mixed solution of maleic anhydride and diphenyl ketone, ultraviolet initiating reaction, filtering, washing and drying to obtain crude fiber grafted with maleic anhydride.
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