CN112011121B - Preparation method of thermoplastic resin-based composite material - Google Patents
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Abstract
The invention provides a preparation method of a thermoplastic resin matrix composite, which comprises the following raw materials in parts by mass: 100 parts of polypropylene, 20-40 parts of chopped glass fiber and 2-3 parts of nano mullite. According to the thermoplastic resin-based composite material and the preparation method thereof, the polypropylene is subjected to addition modification by adopting the nano mullite and the chopped glass fiber, and the tensile property of the polypropylene matrix is greatly improved by adding the reinforcing item, so that the strength of the polypropylene matrix is greatly enhanced.
Description
Technical Field
The invention relates to a preparation method of a thermoplastic resin matrix composite material.
Background
The thermoplastic resin matrix composite material is a composite material which adopts a high-performance reinforcing material to reinforce thermoplastic resin. Compared with the traditional material, the composite material has the characteristics of designability of performance, identity of the material and the structure, composite effect, dependence of material performance on a composite process and the like, and thus has the outstanding advantages of high hardness, high specific strength, high specific stiffness, good damping and shock absorption, high breakage safety and the like. Thermoplastic composites are attracting much attention for their unique properties and are becoming increasingly useful. The technology of thermoplastic composite materials mainly focuses on the following two aspects: 1) A reasonable composite process; 2) Designing an interface layer. At present, thermoplastic composite materials have been widely applied in aerospace, such as parts of adjustable stator blade bushings, liners, large and small cover plates and the like of gas compressors.
The modification research on the thermoplastic composite material is a hot point of research, and the invention provides a novel raw material proportion and a preparation process of the thermoplastic composite material so as to achieve the optimal modification effect.
Disclosure of Invention
The invention aims to provide a thermoplastic resin matrix composite material and a preparation method thereof, so as to achieve the purpose of improving the mechanical property of the resin matrix composite material.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a thermoplastic resin matrix composite material which comprises the following raw materials in parts by mass: 100 parts of polypropylene, 20-40 parts of chopped glass fiber and 2-3 parts of nano mullite.
In the technical scheme, the nano mullite and the chopped glass fiber are adopted to modify the polypropylene, and the tensile property of the polypropylene matrix is greatly improved by adding the reinforcing item, so that the strength of the polypropylene matrix is greatly enhanced.
Preferably, the composite material comprises the following raw materials in parts by mass: based on 100 parts of polypropylene, 30 parts of chopped glass fiber and 2.5 parts of nano mullite.
In the technical scheme, the tensile strength of the composite material prepared according to the proportion is 96.7MPa, which is far higher than that of pure polypropylene by 30MPa.
The invention also provides a preparation method of the thermoplastic resin matrix composite material, which comprises the following steps:
carrying out coupling treatment on the chopped glass fibers by using a silane coupling agent to obtain surface-modified chopped glass fibers;
coupling the nano mullite by using a silane coupling agent to obtain surface-modified nano mullite;
mixing the surface-modified nano mullite, the polypropylene and the surface-modified chopped glass fiber according to the mass ratio of (2-3) to (20-40) to form a mixture;
and carrying out hot press molding on the mixture to form the resin-based composite material.
In the technical scheme, the hot-press molding process is adopted, the formula provided by the preparation method is combined, the strength of the resin-based composite material can still be enhanced by 320%, and meanwhile, compared with injection molding, the process greatly reduces the cost, breaks through the barrier that the injection molding cannot mold a plastic part with large wall thickness variation, and greatly improves the application prospect of a resin-based composite material system.
Preferably, the chopped glass fiber is subjected to coupling treatment by using a silane coupling agent to obtain a surface modified chopped glass fiber; before;
and cleaning the chopped glass fibers.
In the technical scheme, the surface cleaning treatment is carried out before the coupling treatment is carried out on the chopped glass fiber, so that the surface modification effect of the chopped glass fiber can be improved.
Preferably, the chopped glass fibers are subjected to a cleaning process comprising the steps of:
putting the chopped glass fibers into a furnace, keeping the temperature of 400 ℃ for 2 hours, and removing slurry on the surfaces of the chopped glass fibers to obtain primarily clean chopped glass fibers;
preparing a cleaning solution, wherein the molar ratio of NaC1O to CH3COOH of the cleaning solution is 1;
soaking the chopped glass fiber after primary cleaning into the cleaning solution, putting the chopped glass fiber into a 45 ℃ oven, and drying for 16 hours and then taking out the chopped glass fiber;
and repeatedly washing the chopped glass fibers taken out of the oven with distilled water.
In the technical scheme, the chopped glass fiber can achieve a better cleaning effect through primary cleaning, deep cleaning and twice cleaning.
Preferably, the chopped glass fiber is subjected to coupling treatment by using a silane coupling agent to obtain a surface modified chopped glass fiber; the method comprises the following steps:
putting the chopped glass fibers into an absolute ethyl alcohol solution of 1% of silane coupling agent, and immersing the chopped glass fibers in the absolute ethyl alcohol solution;
immersing the chopped glass fibers in the absolute ethyl alcohol solution for 30-60 s, taking out the chopped glass fibers, and drying the chopped glass fibers for 6 hours at the temperature of 120 ℃;
and crushing the dried chopped glass fiber to obtain the surface modified chopped glass fiber.
In the technical scheme, the surface adhesiveness of the chopped glass fiber is improved by coupling the chopped glass fiber, and a better adhesive effect can be achieved in the subsequent hot-press forming process.
Preferably, the nano mullite is subjected to coupling treatment by using a silane coupling agent to obtain surface-modified nano mullite; before;
and drying the nano mullite.
In the technical scheme, the nano mullite is dried before being coupled, so that the surface modification effect of the nano mullite can be improved.
Preferably, the drying treatment is carried out on the nano mullite, and comprises the following steps:
and drying the nano mullite at 105 ℃ for 2 hours to remove the water adsorbed on the surface.
In the technical scheme, the nano mullite can reach the required drying grade through the drying treatment.
Preferably, the nano mullite is subjected to coupling treatment by using a silane coupling agent to obtain surface-modified nano mullite; the method comprises the following steps:
putting a silane coupling agent into absolute ethyl alcohol to prepare an absolute ethyl alcohol solution, and adding nano mullite into the absolute ethyl alcohol solution while stirring to prepare a suspension;
putting the suspension into a water bath, and volatilizing ethanol in the suspension under the action of magnetic stirring;
and (3) drying the suspension liquid volatilized from the ethanol in a drying oven at 105 ℃ to obtain the nano mullite containing 2% of the silane coupling agent.
According to the technical scheme, the nano mullite is subjected to coupling treatment, so that the surface adhesiveness of the nano mullite is improved, and a better adhesion effect can be achieved in the subsequent hot press forming process.
Preferably, mixing the surface-modified nano mullite, the polypropylene and the surface-modified chopped glass fiber according to the mass ratio of (2-3) to (20-40) 100 to form a mixture; the method comprises the following steps:
putting the surface modified nano mullite, the polypropylene and the surface modified chopped glass fiber into an internal mixer according to the mass ratio of (2-3) to (20-40) of 100;
and at room temperature, the internal mixer mixes the nano mullite, the polypropylene and the chopped glass fiber at the speed of 40 r/min for more than 30 minutes to form the mixture.
In the technical scheme, the internal mixer is used for fully mixing the nano mullite, the polypropylene and the chopped glass fiber.
Preferably, the hot press molding of the mixture to form the resin-based composite material comprises the following steps:
putting the mixture into a flat vulcanizing machine, and carrying out hot press molding on the mixture, wherein the hot press temperature is set to 180 ℃, the pressure is set to 0.3GPa, and the pressure maintaining time is more than 8 minutes to form the resin-based composite material;
air cooling the resin matrix composite material subjected to hot press molding for 2 hours;
and demolding the cooled resin-based composite material.
In the technical scheme, the press vulcanizer is used, the mixture can be subjected to hot press molding, and the strength of the resin matrix composite material is greatly enhanced.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The positive progress effects of the invention are as follows:
according to the thermoplastic resin-based composite material and the preparation method thereof, the polypropylene is subjected to addition modification by adopting the nano mullite and the chopped glass fiber, and the tensile property of the polypropylene matrix is greatly improved by adding the reinforcing item, so that the strength of the polypropylene matrix is greatly enhanced.
Drawings
FIG. 1 is a schematic illustration of the fracture morphology of a thermoplastic resin-based composite material formulated in the mass ratio of example 4 according to the present invention.
FIG. 2 is an enlarged schematic view of the fracture morphology of the composite material shown in FIG. 1.
FIG. 3 is a schematic illustration of the fracture morphology of the thermoplastic resin-based composite material formulated in the mass ratio of example 5 according to the present invention.
FIG. 4 is an enlarged schematic view of the fracture morphology of the composite material shown in FIG. 3.
Detailed Description
The invention is further described in the following description with reference to specific embodiments and the accompanying drawings, in which more details are set forth to provide a thorough understanding of the invention, but it will be apparent that the invention can be practiced in many other ways than those specifically described herein, and that a person skilled in the art can make similar generalizations and deductions as to the practice of the invention without departing from the spirit of the invention, and therefore the scope of the invention should not be limited by the contents of this specific embodiment.
The invention provides a thermoplastic resin matrix composite material which comprises the following raw materials in parts by mass: 100 parts of polypropylene, 20-40 parts of chopped glass fiber and 2-3 parts of nano mullite.
The main components of the nano mullite are 3 Al2O3.2SiO2 or 2 Al2O3.SiO2, the nano mullite (content is 90-95 percent) is rod-shaped, the diameter is 30-50 nm, the length is 70-80 nm, and the balance is nano silicon dioxide (cristobalite), the shape is nearly spherical, and the diameter is 5-10 nm.
Wherein the chopped glass fiber is formed by on-line chopping of strand drawn by a special impregnating compound through a wet method. The chopped glass fiber used in the experiment is about 0.01-0.02 mm and is obtained by crushing centimeter-level glass fiber by a high-speed crusher.
The invention adopts nano mullite and chopped glass fiber to add and modify polypropylene, researches the rheological property of the composite material through a torque rheometer, tests the mechanical property of the composite material through a universal tester, and analyzes the fracture morphology of the composite material through a scanning electron microscope.
A torque rheometer is adopted to perform rheological analysis on pure polypropylene, polypropylene-based composite materials containing 2.5 percent and 3 percent of nano-mullite and polypropylene-based composite materials containing 2.5 percent of nano-mullite and 20 percent, 30 percent and 40 percent of chopped glass fiber respectively.
The experiment shows that: with the addition of the nano mullite, the feeding peak value (maximum torque) is reduced, the balance torque is also reduced, the nano mullite has a good plasticizing effect on the polypropylene, and the higher the content of the nano mullite is, the lower the feeding peak value is, but the balance torque is slightly increased, which indicates that the increase of the addition amount of the nano mullite cannot play a role in increasing the plasticity of the polypropylene to a greater extent. With the increase of the chopped glass fibers, the melting time and the equilibrium time of the polypropylene are shortened, which is beneficial to improving the melting speed of the polypropylene; the maximum torque and equilibrium torque of the composite increased significantly indicating that the addition of chopped glass fibers affected the flowability of the composite.
The invention adopts an analysis method of an orthogonal test, selects 2 factors of the dosage of the nano mullite and the chopped glass fiber, sets each factor at 3 levels, and respectively takes the tensile strength, the elongation and the Shore hardness value as indexes, wherein 100g of polypropylene is fixed in the preparation process. Performing sample preparation test and performance test, and finally determining the optimal mixture ratio as follows: chopped glass fiber/nano mullite/polypropylene =30/2.5/100 (mass ratio). Namely, the composite material comprises the following raw materials in parts by mass: based on 100 parts of polypropylene, 30 parts of chopped glass fiber and 2.5 parts of nano mullite. The tensile strength of the composite material prepared according to the proportion is 96.7MPa, which is far higher than that of pure polypropylene by 30MPa.
The preparation method of the thermoplastic resin-based composite material is as follows. The preparation methods of examples 1 to 11 were the same, except that the proportions of nano mullite, polypropylene and chopped glass fiber were different, and the proportions are shown in table 1.
Specifically, the preparation method of the thermoplastic resin-based composite material comprises the following steps:
1) Cleaning the chopped glass fibers;
2) Carrying out coupling treatment on the chopped glass fibers by using a silane coupling agent to obtain surface-modified chopped glass fibers;
3) Drying the nano mullite;
4) Coupling the nano mullite by using a silane coupling agent to obtain surface-modified nano mullite;
5) Mixing the surface-modified nano mullite, the polypropylene and the surface-modified chopped glass fiber according to a certain mass ratio (the mass ratio is shown in Table 1) to form a mixture;
6) And carrying out hot press molding on the mixture to form the resin-based composite material.
The preparation method adopts a hot-press forming process, and researches show that the formula provided by the preparation method is combined with the hot-press forming process, so that the strength of the resin-based composite material can still be enhanced by 320 percent.
Wherein, the step 1) of cleaning the chopped glass fiber comprises the following steps:
11 Placing the chopped glass fibers into a furnace, keeping the temperature of the furnace at 400 ℃ for 2 hours, and removing the sizing agent on the surfaces of the chopped glass fibers to obtain the primarily clean chopped glass fibers;
12 Preparing a cleaning solution, wherein the molar ratio of NaC1O to CH3COOH of the cleaning solution is 1; the volume of the cleaning solution is prepared according to the quantity of the chopped glass fibers to be treated each time;
13 Soaking the chopped glass fiber after primary cleaning into the cleaning solution, putting the chopped glass fiber into a 45 ℃ oven, drying for 16 hours, and taking out;
14 The chopped glass fibers removed from the oven were repeatedly rinsed clean with distilled water.
Wherein, the step 2) is to carry out coupling treatment on the chopped glass fiber by using a silane coupling agent to obtain the surface modified chopped glass fiber; the method comprises the following steps:
21 Placing the chopped glass fibers into an absolute ethyl alcohol solution of 1% of silane coupling agent, and immersing the chopped glass fibers in the absolute ethyl alcohol solution;
22 ) immersing the chopped glass fiber in an absolute ethyl alcohol solution for 30-60 s, then taking out the chopped glass fiber, and drying the chopped glass fiber for 6 hours at the temperature of 120 ℃;
23 The dried chopped glass fibers are crushed to obtain surface-modified chopped glass fibers.
Wherein, the step 3) of drying the nano mullite comprises the following steps: and drying the nano mullite at 105 ℃ for 2 hours to remove the water adsorbed on the surface.
Wherein, the step 4) is to carry out coupling treatment on the nano mullite by using a silane coupling agent to obtain the surface modified nano mullite; the method comprises the following steps:
41 Putting the silane coupling agent into absolute ethyl alcohol to prepare absolute ethyl alcohol solution, and adding the nano mullite into the absolute ethyl alcohol solution while stirring to prepare suspension;
42 Putting the suspension into a water bath, and volatilizing the ethanol in the suspension under the action of magnetic stirring;
43 The suspension liquid volatilized by the ethanol is put into a drying oven at 105 ℃ for drying, and the nano mullite containing 2 percent of silane coupling agent is obtained.
Step 5) mixing the surface-modified nano mullite, the polypropylene and the surface-modified chopped glass fiber according to a certain mass ratio (mass ratio is shown in Table 1) to form a mixture; the method comprises the following steps:
51 Putting the surface-modified nano mullite, the polypropylene and the surface-modified chopped glass fiber into an internal mixer according to a certain mass ratio (the mass ratio is shown in table 1);
52 At room temperature, the nano mullite, the polypropylene and the chopped glass fiber are mixed by an internal mixer at the speed of 40 r/min for more than 30 minutes to form a mixture.
Wherein, step 6) carries on the hot briquetting to the mixture, form the resin matrix composite, including the following steps:
61 Putting the mixture into a flat vulcanizing machine, and carrying out hot press molding on the mixture, wherein the hot press temperature is set to 180 ℃, the pressure is set to 0.3GPa, and the pressure maintaining time is more than 8 minutes, so as to form the resin-based composite material;
62 Air cooling the resin-based composite material after hot press molding for 2 hours;
63 Demolding the cooled resin-based composite material.
Performing performance tests on the composite materials prepared in the above examples 1 to 9, wherein the tensile properties of the composite materials are tested by adopting a tensile sample machine, the test sample adopts a standard tensile sample, the test speed is 5mm/min, and the tensile force is 2KN; the hardness of the composite material is measured by an XHS type Shore D rubber and plastic hardness tester; a material torque-time change curve made by a torque rheometer can analyze the whole plasticizing process from feeding to melting to decomposition (crosslinking) of the plastic according to the magnitude of a torque value in the curve, the time of occurrence of a peak value, the shape of the curve and the like; the fracture morphology of the composite material is observed and analyzed by a scanning electron microscope of S-3000N type of Hitachi, japan.
The mass ratios and mechanical properties of the above examples 1 to 9 are shown in Table 1.
TABLE 1 EXAMPLES 1-9 Mass ratios and mechanical Properties
As can be seen from the comparative research results in the above examples, the addition of the reinforcing term greatly improves the tensile strength of the polypropylene matrix, the tensile strength of the polypropylene can only reach 30MPa or a little higher level, and the dual-phase reinforcement increases the strength of the matrix by 320%. The most preferred enhanced formulation is example 5: nano mullite: polypropylene: chopped glass fibers (mass ratio) =2.5:100:30.
fracture morphology analysis is respectively carried out on the composite materials prepared in the examples 4 and 5 of the patent of the invention, fig. 1 and 2 are fracture morphology of the example 4, fig. 3 and 4 are fracture morphology of the example 5, wherein the gray floccule is a polypropylene matrix, and the rod-shaped object is a glass fiber, so that it can be seen that the glass fiber of the example 4 is not completely contacted with the polypropylene matrix, which indicates that the infiltration effect of the matrix and the glass fiber is not ideal, and the fracture morphology of the sample of the example 5 is observed, so that the glass fiber amount is higher than that of the example 4, the distribution is more uniform, the sharp decrease of the pore amount is obviously seen, which indicates that the combination of the polypropylene matrix and the glass fiber is better, and the load transmission effect of the glass fiber can be effectively exerted.
Although the present invention has been disclosed in terms of the preferred embodiment, it is not intended to limit the invention, and variations and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention. Any modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the scope of protection defined by the claims of the present invention, unless departing from the content of the technical solution of the present invention.
Claims (10)
1. The preparation method of the thermoplastic resin-based composite material is characterized by comprising the following raw materials in parts by mass: 100 parts of polypropylene, 20-40 parts of chopped glass fiber and 2-3 parts of nano mullite, and the preparation method of the thermoplastic resin-based composite material comprises the following steps:
carrying out coupling treatment on the chopped glass fibers by using a silane coupling agent to obtain surface-modified chopped glass fibers;
coupling the nano mullite by using a silane coupling agent to obtain surface-modified nano mullite;
mixing the surface-modified nano mullite, the polypropylene and the surface-modified chopped glass fiber according to the mass ratio of (2-3) to (20-40) to form a mixture;
and carrying out hot press molding on the mixture to form the resin-based composite material.
2. The method for preparing the thermoplastic resin-based composite material according to claim 1, wherein the composite material comprises the following raw materials in parts by mass: based on 100 parts of polypropylene, the chopped glass fiber accounts for 30 parts, and the nano mullite accounts for 2.5 parts.
3. The method of preparing a thermoplastic resin-based composite material according to claim 1, characterized in that: carrying out coupling treatment on the chopped glass fiber by using a silane coupling agent to obtain a surface modified chopped glass fiber; before;
and cleaning the chopped glass fibers.
4. The method for preparing a thermoplastic resin-based composite material according to claim 3, wherein the cleaning of the chopped glass fibers comprises the following steps:
putting the chopped glass fibers into a furnace, keeping the temperature at 400 ℃ for 2 hours, and removing slurry on the surfaces of the chopped glass fibers to obtain primarily clean chopped glass fibers;
preparing a cleaning solution, wherein the molar ratio of NaC1O to CH3COOH of the cleaning solution is 1;
soaking the chopped glass fiber after primary cleaning into the cleaning solution, putting the chopped glass fiber into a 45 ℃ oven, and drying for 16 hours and then taking out the chopped glass fiber;
and repeatedly washing the chopped glass fibers taken out of the oven with distilled water.
5. The method for preparing a thermoplastic resin-based composite material according to claim 1, wherein the chopped glass fibers are subjected to coupling treatment using a silane coupling agent to obtain surface-modified chopped glass fibers; the method comprises the following steps:
putting the chopped glass fibers into an absolute ethyl alcohol solution of 1% of silane coupling agent, and immersing the chopped glass fibers in the absolute ethyl alcohol solution;
immersing the chopped glass fibers in the absolute ethyl alcohol solution for 30-60 s, taking out the chopped glass fibers, and drying the chopped glass fibers for 6 hours at the temperature of 120 ℃;
and crushing the dried chopped glass fiber to obtain the surface modified chopped glass fiber.
6. The method for preparing the thermoplastic resin-based composite material according to claim 1, wherein the nano mullite is subjected to coupling treatment by using a silane coupling agent to obtain surface-modified nano mullite; before;
and drying the nano mullite.
7. The method for preparing a thermoplastic resin-based composite material according to claim 6, wherein the drying treatment of the nano mullite comprises the following steps:
and drying the nano mullite at 105 ℃ for 2 hours to remove the water adsorbed on the surface.
8. The method for preparing the thermoplastic resin-based composite material according to claim 1, wherein the nano mullite is subjected to coupling treatment by using a silane coupling agent to obtain surface-modified nano mullite; the method comprises the following steps:
putting a silane coupling agent into absolute ethyl alcohol to prepare an absolute ethyl alcohol solution, and adding nano mullite into the absolute ethyl alcohol solution while stirring to prepare a suspension;
putting the suspension into a water bath, and volatilizing ethanol in the suspension under the action of magnetic stirring;
and (3) drying the suspension liquid volatilized from the ethanol in a drying oven at 105 ℃ to obtain the nano mullite containing 2% of the silane coupling agent.
9. The preparation method of the thermoplastic resin-based composite material is characterized in that the surface-modified nano mullite, the polypropylene and the surface-modified chopped glass fiber are mixed according to the mass ratio of (2-3) to (100) (20-40) to form a mixture; the method comprises the following steps:
putting the surface-modified nano mullite, the polypropylene and the surface-modified chopped glass fiber into an internal mixer according to the mass ratio of (2-3) to (20-40) of 100;
and at room temperature, the internal mixer mixes the nano mullite, the polypropylene and the chopped glass fiber at the speed of 40 r/min for more than 30 minutes to form the mixture.
10. The method for preparing a thermoplastic resin-based composite material according to claim 1, wherein the step of hot-press forming the mixed material to form a resin-based composite material comprises the steps of:
putting the mixture into a flat vulcanizing machine, and carrying out hot press molding on the mixture, wherein the hot press temperature is set to 180 ℃, the pressure is set to 0.3GPa, and the pressure maintaining time is more than 8 minutes to form the resin-based composite material;
air cooling the resin-based composite material subjected to hot press molding for 2 hours;
and demolding the cooled resin-based composite material.
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