Method for preparing carbon fiber reinforced thermoplastic resin-based felt and composite material by suspension blending method

Abstract

The present invention discloses a method for preparing carbon fiber reinforced thermoplastic resin-based felt and composite materials by a suspension blending method, and belongs to the field of carbon fiber composite materials. In the present invention, the suspension is prepared by using a carbon fiber surface modifier, nanoparticles and a non-ionic surfactant in proportion; the de-sizing carbon fiber and the thermoplastic resin fiber are placed in the prepared suspension, and the suspension not only realizes the surface modification of the carbon fiber, but also provides a dispersion environment for the carbon fiber and the resin fiber. The suspension box is equipped with relative blades to stir the resin fiber and the carbon fiber under the action of turbulence, and an ultrasonic vibration device is provided to assist the uniform dispersion of the fiber to obtain a slurry; the slurry in the suspension box is taken out by a container, and is placed in a filter, and a thin layer of felt is obtained after filtering the solution; the thin felt is stacked layer by layer to a certain thickness, and acupuncture is performed after drying to obtain a carbon fiber reinforced thermoplastic resin-based felt; and the felt is then hot-pressed to obtain its composite material.

Description

Technical Field

[0001] The invention belongs to the field of carbon fiber composite materials, and specifically relates to a method for preparing a carbon fiber reinforced thermoplastic resin-based felt material and a composite material by a suspension blending method. Background Art

[0002] Carbon fiber modified reinforced composite material is a new type of lightweight, high-strength material with good properties of corrosion resistance and excellent mechanical properties. In recent years, the manufacture of carbon fiber composite materials has provided a harder and lighter alternative to traditional metal parts. In the automotive industry, the application of carbon fiber reinforced composite materials is becoming more and more extensive.

[0003] At present, fiber-reinforced composite materials have defects such as uneven distribution of reinforcing fibers in the resin matrix, which greatly affects the performance of the material. Traditional fiber-reinforced resin materials also have the defects of complex processes and high prices. Taking traditional carbon fiber reinforced resin as an example, its preparation method includes: 1) carbon fiber felt molding; 2) resin impregnation into prepreg; 3) prepreg hot pressing molding. The high price limits the large-scale application of fiber-reinforced resin materials.

[0004] Aiming at the main shortcomings of current carbon fiber reinforced thermoplastic composites, such as uneven distribution of reinforcing fibers in the resin matrix and defects in the interface between reinforcing fibers and resin, a suspension blending method was proposed to achieve uniform blending of carbon fibers and resin fibers with large density differences, and to prepare low-cost, high-performance carbon fiber reinforced thermoplastic resin-based composites. Summary of the invention

[0005] In order to overcome the above-mentioned shortcomings, the purpose of the present invention is to provide a method for preparing a carbon fiber reinforced thermoplastic resin-based felt material and a composite material by a suspension blending method. The present invention adopts the following technical scheme:

[0006] A method for preparing a carbon fiber reinforced thermoplastic resin-based felt material and a composite material by a suspension blending method, comprising the following steps:

[0007] 1) Preparation of suspension: ethanol and deionized water were mixed in a mass ratio of 95:5 as a solvent to dissolve the modifier to obtain a solution with a concentration of 3 wt%, and mechanically stirred and treated with an ultrasonic device for 30 min, and then 0.2% of the solution mass of nanoparticles, 0.125% of Triton X-100 and 1.25% of PEG-100000 were added, and mechanically stirred and treated with an ultrasonic device for 30-60 min to obtain a stable suspension;

[0008] 2) firstly putting the resin fiber into the suspension, and then putting the desizing carbon fiber into the suspension, stirring the two fibers uniformly by two sets of relative blades to form turbulence and assisting with ultrasonic device, and the mixing treatment time is 30 minutes to obtain a slurry, wherein the mass concentration of the total fiber of the resin fiber and the carbon fiber in the slurry is 0.01wt%-5wt%, and the carbon fiber or the resin fiber accounts for 20%-80% of the total fiber content;

[0009] 3) Using a container to take out the slurry and putting it into a filter to obtain a thin layer of carbon fiber reinforced thermoplastic resin-based felt, each layer of thin carbon fiber reinforced thermoplastic resin-based felt has a thickness of 3-5 mm, and then taking several layers of thin carbon fiber reinforced thermoplastic resin-based felt, stacking them together, putting them into a drying oven at a temperature of 100-200° C., and after acupuncture, obtaining a carbon fiber reinforced thermoplastic resin-based felt;

[0010] 4) hot pressing the carbon fiber reinforced thermoplastic resin-based felt to obtain a carbon fiber reinforced thermoplastic resin-based composite material; the hot pressing conditions are hot pressing temperature of 110-400° C. and hot pressing time of 0.5-10 min.

[0011] The modifier is one or a combination of KH550, KH560, KH570, N-methylpyrrolidone, and maleic anhydride;

[0012] The nanoparticles are one or a combination of carbon nanotubes, nano silicon dioxide, and graphene oxide;

[0013] The carbon fiber is one or a combination of PAN-based carbon fiber, asphalt-based carbon fiber, viscose-based carbon fiber, and recycled carbon fiber;

[0014] The resin fiber is one or a combination of nylon fiber, polyetheretherketone fiber, polypropylene fiber, polylactic acid fiber and ultra-high molecular weight fiber;

[0015] The length of the resin fiber is 30-80 mm, preferably 50 mm, the fineness of the resin fiber is 0.1-0.7 dtex, preferably 0.5 dtex. The length of the carbon fiber is 30-60 mm, preferably 40 mm.

[0016] The thickness of the carbon fiber reinforced thermoplastic resin matrix composite material is 0.1-10 mm.

[0017] The preparation process of desizing carbon fiber is as follows:

[0018] A mixed solvent was prepared by taking acetone and ethanol in a volume ratio of 1:1, the carbon fiber was placed in the mixed solvent and stirred mechanically for 30 minutes, washed with a 0.4wt% sodium hydroxide solution, the carbon fiber tow was taken out and placed in a drying oven, and dried at 120°C for 30 minutes.

[0019] Beneficial effects of the present invention:

[0020] The present invention adopts integrated material taking to ensure that the concentration of the slurry in the suspension box is uniform, and the filtered suspension can be recycled and reused. The prepared carbon fiber reinforced thermoplastic resin-based composite material has good tensile properties, bending properties, impact properties, antistatic properties, good interface compatibility, and uniform distribution of reinforced fibers and resin matrix. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 The invention discloses a method for preparing a carbon fiber reinforced thermoplastic resin-based felt material and a composite material by a suspension blending method.

[0022] Among them: 1-carbon fiber; 2-agitator; 3-de-sizing agent; 4-drying box; 5-square gauze; 6-resin fiber; 7-de-sizing carbon fiber; 8-paddle blades; 9-suspension blending box; 10-ultrasonic device; 11-mold; 12-filter screen; 13-filtrate collection device; 14-needle punching; 15-drying box; 16-hot molding DETAILED DESCRIPTION

[0023] The present invention is further described in detail below in conjunction with examples, but the embodiments of the present invention are not limited thereto. The reagents and materials used in the following examples, unless otherwise specified, are all commercially available products.

[0024] Example 1 (20 wt% carbon fiber, 72 wt% polyetheretherketone fiber, 8 wt% ultra-high molecular weight polyethylene fiber)

[0025] Step a: desizing carbon fiber: prepare a mixed solvent of acetone and ethanol in a volume ratio of 1:1, put the carbon fiber into the solution and stir it with a propeller stirrer for 30 minutes, wash it with a low concentration sodium hydroxide solution (generally with a concentration of 0.4wt%), take out the carbon fiber tow and put it into a drying box, set the drying temperature to 120°C; dry it for 30 minutes to obtain desizing carbon fiber.

[0026] Step b: Preparation of suspension: Prepare a mixed solvent according to the mass ratio of ethanol and deionized water of 95:5, dissolve KH560 in the mixed solvent to a concentration of 3wt%, use relative blade stirring and ultrasonic device to assist in dispersion for 30min, then add 0.2% carbon nanotubes, 0.125% Triton X-100 and 1.25% PEG-100000 by mass of the mixed solution, and then use relative blade stirring and ultrasonic device to assist in dispersion for 30min.

[0027] Step c: mixing carbon fiber reinforced fibers in a suspension: according to fiber density, first put 100.8 g of polyetheretherketone fiber with the lowest density into 14000 g of suspension, then put 28 g of carbon fiber and 11.2 g of ultra-high molecular weight polyethylene fiber into the suspension, stir with two sets of relative blades to form turbulence and use an ultrasonic device to assist in uniformly mixing the fibers, process for 30 minutes, and obtain a slurry.

[0028] Step d: filtering, drying, and molding: taking out the slurry from a fixed container and putting it into a filter to obtain a thin layer of carbon fiber reinforced thermoplastic resin-based felt, each layer of thin carbon fiber reinforced thermoplastic resin-based felt having a thickness of 5 mm, and then stacking five layers of thin carbon fiber reinforced thermoplastic resin-based felt together, placing them in a drying oven and drying them at 120° C. for 10 min, and then performing needle punching with a needle punching machine to obtain a carbon fiber reinforced thermoplastic resin-based felt;

[0029] The carbon fiber reinforced thermoplastic resin-based felt material is then placed in a molding machine for hot pressing molding, wherein the molding temperature is 395° C. and the hot pressing time is 3 minutes, thereby obtaining a carbon fiber reinforced thermoplastic resin-based composite material.

[0030] Example 2 (40 wt% carbon fiber, 54 wt% polyetheretherketone, 6 wt% ultra-high molecular weight polyethylene fiber).

[0031] Step a: desizing carbon fiber: in step a, acetone and ethanol are prepared into a mixed solvent in a volume ratio of 1:1, the carbon fiber is placed in the solution and stirred for 30 minutes with a propeller stirrer, and the carbon fiber is washed with a low concentration sodium hydroxide solution, the carbon fiber tow is taken out and placed in a drying box, and the drying temperature is set to 150° C.; the drying time is 30 minutes to obtain desizing carbon fiber.

[0032] Step b: Preparation of suspension: Prepare a mixed solvent according to the mass ratio of ethanol and deionized water of 95:5, dissolve KH560 in the mixed solvent to a concentration of 3wt%, use relative blade stirring and ultrasonic device to assist in dispersion for 30min, then add 0.2% carbon nanotubes, 0.125% Triton X-100 and 1.25% PEG-100000 by mass of the mixed solution, and then use relative blade stirring and ultrasonic device to assist in dispersion for 30min.

[0033] Step c: mixing carbon fiber reinforced fibers in a suspension: first, putting 83.16 g of polyetheretherketone fiber into 14,000 g of a suspension, and then putting 75.6 g of carbon fiber and 9.24 g of ultra-high molecular weight polyethylene fiber into the suspension, stirring with two sets of opposing blades to form turbulence and using an ultrasonic device to assist in uniformly mixing the fibers, and treating for 30 minutes to obtain a slurry.

[0034] Step d: filtering, drying, and molding: taking out the slurry from a fixed container and putting it into a filter to obtain a thin layer of carbon fiber reinforced thermoplastic resin-based felt, each layer of which has a thickness of 3 mm, and then stacking seven layers of felt together, putting them into a drying oven and drying them at 120° C. for 10 min, and then needle-punching them with a needle-punching machine to obtain a carbon fiber reinforced thermoplastic resin-based felt;

[0035] The carbon fiber reinforced thermoplastic resin-based felt material is then placed in a molding machine for hot pressing molding, wherein the molding temperature is 395° C. and the hot pressing time is 3 minutes, thereby obtaining a carbon fiber reinforced thermoplastic resin-based composite material.

[0036] Example 3 (50 wt% carbon fiber, 44 wt% polyetheretherketone, 6 wt% ultra-high molecular weight polyethylene)

[0037] Step a: desizing carbon fiber: Step a: prepare a mixed solvent of acetone and ethanol in a volume ratio of 1:1, put the carbon fiber into the solution and stir it with a propeller stirrer for 30 minutes, wash it with a low concentration sodium hydroxide solution, take out the carbon fiber tow and put it into a drying box, set the drying temperature to 200°C; dry it for 20 minutes to obtain desizing carbon fiber.

[0038] Step b: Preparation of suspension: Prepare a mixed solvent according to the mass ratio of ethanol and deionized water of 95:5, dissolve KH560 in the mixed solvent to a concentration of 3wt%, use relative blade stirring and ultrasonic device to assist in dispersion for 30min, then add 0.2% carbon nanotubes, 0.125% Triton X-100 and 1.25% PEG-100000 by mass of the mixed solution, and then use relative blade stirring and ultrasonic device to assist in dispersion for 30min.

[0039] Step c: mixing carbon fiber reinforced fibers in a suspension: first, putting 55.44 g of polyetheretherketone fiber into 14,000 g of a suspension, and then putting 63.0 g of carbon fiber and 7.56 g of ultra-high molecular weight polyethylene into the suspension, stirring with two sets of opposing blades to form turbulence and using an ultrasonic device to assist in uniformly mixing the fibers, and treating for 30 minutes to obtain a slurry.

[0040] Step d: filtering, drying, and molding: taking out the slurry from a fixed container and putting it into a filter to obtain a thin layer of carbon fiber reinforced thermoplastic resin-based felt, each layer of thin carbon fiber reinforced thermoplastic resin-based felt having a thickness of 4 mm, and then stacking six layers of thin carbon fiber reinforced thermoplastic resin-based felt together, placing them in a drying oven and drying them at 120° C. for 10 min, and then performing needle punching with a needle punching machine to obtain a carbon fiber reinforced thermoplastic resin-based felt;

[0041] The carbon fiber reinforced thermoplastic resin-based felt material is then placed in a molding machine for hot pressing molding, wherein the molding temperature is 395° C. and the hot pressing time is 3 minutes, thereby obtaining a carbon fiber reinforced thermoplastic resin-based composite material.

[0042] In the above embodiment, the thickness of the carbon fiber reinforced thermoplastic resin-based composite material obtained after hot pressing is 1-10 mm.

[0043] In the above embodiment, the length of the resin fiber is 30-80 mm, preferably 50 mm. The fineness of the resin fiber is 0.1-0.7 dtex, preferably 0.5 dtex. The length of the carbon fiber is 30-60 mm, preferably 40 mm.

[0044] The steps adopted by the present invention include desizing and modifying carbon fibers, preparing a suspension, preparing a carbon fiber reinforced thermoplastic resin-based felt material by a suspension blending method, and obtaining a carbon fiber reinforced thermoplastic resin-based composite material by hot pressing.

[0045] The suspension is prepared by using a carbon fiber surface modifier, nanoparticles and a non-ionic surfactant in proportion, desizing carbon fiber and resin fiber are put into the prepared suspension, relative blades are stirred in a suspension box to make the resin fiber and the carbon fiber evenly mixed under the action of turbulence, and an ultrasonic vibration device assists in the dispersion of the fibers, the slurry in the suspension is taken out by using a container and put into a filter, and the solution is filtered to obtain a thin carbon fiber reinforced thermoplastic resin-based felt material, the thin carbon fiber reinforced thermoplastic resin-based felt material is stacked layer by layer to obtain a certain thickness, dried, and needle-punched to obtain a carbon fiber reinforced thermoplastic resin-based felt material, and then hot-pressed to obtain a carbon fiber reinforced thermoplastic resin-based composite material.

[0046] Effect verification

[0047] Table 1 shows the performance test data of the carbon fiber reinforced thermoplastic resin-based composite materials prepared in Examples 1-3.

[0048]

[0049] It can be seen from Table 1 that the carbon fiber reinforced thermoplastic resin-based composite material prepared by the method of the present invention has good tensile properties, bending properties, impact properties, antistatic properties, good interface compatibility, and uniform distribution of the reinforcing fibers and the resin matrix.

Claims

1. A method for preparing a carbon fiber reinforced thermoplastic resin-based felt material by a suspension blending method, characterized in that: The steps of this method are as follows: 1) Preparation of suspension: ethanol and deionized water are mixed as a solvent in a mass ratio of 95:5, and a modifier is dissolved to obtain a solution with a concentration of 3wt%, and the solution is mechanically stirred and treated with an ultrasonic device for 30 minutes, and then 0.2% of the solution mass of nanoparticles, 0.125% of Triton X-100 and 1.25% of PEG-100000 are added, and the solution is mechanically stirred and treated with an ultrasonic device for 30-60 minutes to obtain a stable suspension; the modifier is one or a combination of KH550, KH560, KH570, N-methylpyrrolidone, and maleic anhydride; the nanoparticles are one or a combination of carbon nanotubes, nanosilicon dioxide, and graphene oxide; 2) Firstly, the resin fiber is put into the suspension, and then the desizing carbon fiber is put into the suspension, and the two fibers are uniformly mixed by stirring with two sets of relative blades to form turbulence and an ultrasonic device, and the mixing treatment time is 30-60 minutes to obtain a slurry, wherein the mass concentration of the total fiber of the resin fiber and the carbon fiber in the slurry is 0.01wt%-5wt%, and the carbon fiber or the resin fiber accounts for 20%-80% of the total fiber content; the material of the resin fiber is thermoplastic resin; the carbon fiber is one or a combination of PAN-based carbon fiber, asphalt-based carbon fiber, viscose-based carbon fiber, and recycled carbon fiber, and the length of the carbon fiber is 30-60mm; The resin fiber is one or a combination of nylon fiber, polyetheretherketone fiber, polypropylene fiber, polylactic acid fiber and ultra-high molecular weight polyethylene fiber, the resin fiber has a length of 30-80 mm and a fineness of 0.1-0.7 dtex; 3) Use a container to take out the slurry and put it into a filter to obtain a thin layer of carbon fiber reinforced thermoplastic resin-based felt, each layer of thin carbon fiber reinforced thermoplastic resin-based felt is 3-5 mm thick, and then take several layers of thin carbon fiber reinforced thermoplastic resin-based felt and stack them together, put them into a drying oven and dry them at a temperature of 100-200°C, and after needling, hot molding is performed to obtain carbon fiber reinforced thermoplastic resin-based felt.

2. The method for preparing carbon fiber reinforced thermoplastic resin-based felt by a suspension blending method according to claim 1, characterized in that: The process of desizing the carbon fiber in step 1) is as follows: A mixed solvent was prepared by taking acetone and ethanol in a volume ratio of 1:1, the carbon fiber was placed in the mixed solvent and stirred mechanically for 30 minutes, washed with a 0.4wt% sodium hydroxide solution, the carbon fiber tow was taken out and placed in a drying oven, and dried at 120°C for 30 minutes.

3. The method for preparing carbon fiber reinforced thermoplastic resin-based felt by a suspension blending method according to claim 1, characterized in that: The carbon fiber length is 40mm.

4. The method for preparing carbon fiber reinforced thermoplastic resin-based felt by a suspension blending method according to claim 1, characterized in that: The resin fiber length is 50 mm and the fineness is 0.5 dtex.

5. A method for preparing a carbon fiber reinforced thermoplastic resin-based composite material by a suspension blending method, characterized in that: The steps of this method are as follows: 1) Preparation of suspension: ethanol and deionized water are mixed as a solvent in a mass ratio of 95:5, and a modifier is dissolved to obtain a solution with a concentration of 3wt%, and the solution is mechanically stirred and treated with an ultrasonic device for 30 minutes, and then 0.2% of the solution mass of nanoparticles, 0.125% of Triton X-100 and 1.25% of PEG-100000 are added, and the solution is mechanically stirred and treated with an ultrasonic device for 30-60 minutes to obtain a stable suspension; the modifier is one or a combination of KH550, KH560, KH570, N-methylpyrrolidone, and maleic anhydride; the nanoparticles are one or a combination of carbon nanotubes, nanosilicon dioxide, and graphene oxide; 2) Firstly, the resin fiber is put into the suspension, and then the desizing carbon fiber is put into the suspension, and the two fibers are uniformly mixed by stirring with two sets of relative blades to form turbulence and an ultrasonic device, and the mixing treatment time is 30-60 minutes to obtain a slurry, wherein the mass concentration of the total fiber of the resin fiber and the carbon fiber in the slurry is 0.01wt%-5wt%, and the carbon fiber or the resin fiber accounts for 20%-80% of the total fiber content; the material of the resin fiber is thermoplastic resin; the carbon fiber is one or a combination of PAN-based carbon fiber, asphalt-based carbon fiber, viscose-based carbon fiber, and recycled carbon fiber, and the length of the carbon fiber is 30-60mm; The resin fiber is one or a combination of nylon fiber, polyetheretherketone fiber, polypropylene fiber, polylactic acid fiber and ultra-high molecular weight polyethylene fiber, the resin fiber has a length of 30-80 mm and a fineness of 0.1-0.7 dtex; 3) Using a container to take out the slurry and put it into a filter to obtain a thin layer of carbon fiber reinforced thermoplastic resin-based felt, each layer of thin carbon fiber reinforced thermoplastic resin-based felt is 3-5 mm thick, and then several layers of thin carbon fiber reinforced thermoplastic resin-based felt are stacked together, put into a drying oven and dried at a temperature of 100-200° C., and after needling, hot molding is performed to obtain a carbon fiber reinforced thermoplastic resin-based felt; 4) hot pressing the carbon fiber reinforced thermoplastic resin-based felt to obtain a carbon fiber reinforced thermoplastic resin-based composite material; the hot pressing conditions are a hot pressing temperature of 395-400° C. and a hot pressing time of 0.5-10 min.

6. The carbon fiber reinforced thermoplastic resin-based composite material prepared by the method according to claim 5, characterized in that: The carbon fiber reinforced thermoplastic resin-based composite material has a thickness of 0.1-10 mm.

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