CN111844822A - High-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform and preparation method thereof - Google Patents
High-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform and preparation method thereof Download PDFInfo
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- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
Abstract
The invention discloses a high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform and a preparation method thereof. The preparation method comprises the following steps: compounding thermoplastic resin, an auxiliary agent and continuous fibers into a continuous fiber reinforced thermoplastic sheet with the thickness of 0.1-0.2 mm in a melting and dipping mode; cutting the continuous sheet into small pieces with the length and width of (10-50 mm) × (5-10 mm); uniformly mixing the cut small sheets to keep the isotropy of fiber distribution; heating to melt the uniformly mixed small slices; then mixing the fibers by low-shear mixing equipment to enable the fibers to be distributed isotropically; and cold-pressing the compound melt in the molten state into a sheet with a certain width and the thickness of 1-5 mm. Compared with the existing preparation method, the discontinuous fiber reinforced thermoplastic composite material prepared by the invention has better isotropy and higher impact strength.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and relates to a high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform and a preparation method thereof.
Background
There are two main categories of fiber reinforced thermoplastic composites: continuous fiber reinforced thermoplastic Composites (CFRTP) and discontinuous fiber reinforced thermoplastic composites; non-continuous fiber reinforced thermoplastic composites are further classified into three categories: short fiber reinforced thermoplastic composites (SFT), long fiber reinforced thermoplastic composites (LFT), and fiber mat reinforced thermoplastic composites (GMT).
Continuous fiber reinforced thermoplastic Composites (CFRTP) have strength and impact properties comparable to metals, but suffer from poor formability and processability, and low freedom of design of product structure; although the discontinuous fiber reinforced thermoplastic composite materials SFT, LFT and GMT have good molding processability, the impact resistance (notch impact strength) is too low and is far from metal, so that the method is difficult to realize that steel is replaced by plastic in a true sense.
In the related patents of SFT, such as publication No. CN101311222B, the patent application entitled "a high impact fiber reinforced engineering plastic and preparation method", a twin-screw co-extrusion preparation process is used, the tensile strength of which is only 111.1 MPa; the notched impact strength is only 22.2kJ/m2(ii) a For example, in patent application publication No. CN10271907B entitled "a fiber reinforced polycarbonate resin having high impact strength and method for preparing the same", a twin-screw co-extrusion preparation process is employed, the tensile strength of which is only 114.5 MPa; the notched impact strength was only 118.1J/m (about 12 kJ/m) 2) (ii) a For example, in patent application with publication number CN106751765A entitled "a wear-resistant high impact nylon composite material and its preparation method and application", a twin-screw blending extrusion preparation process is adopted, and the tensile strength is only 151MPa at most; the notched impact strength was only 11.9kJ/m2。
In patents related to LFT, such as patent application publication No. CN105273316A entitled "A high impact Long fiber reinforced Polyethylene (PE) composite and method of manufacture", a melt impregnation process is used to produce a composite material having tensile strengthThe highest degree is only 130 MPa; the maximum notch impact strength is only 40kJ/m2(ii) a For example, in patent application publication No. CN 108219287A entitled "a low warpage high impact resistant long fiber reinforced polypropylene composite material and method for preparing the same", a melt impregnation preparation process is adopted, and the tensile strength is only 86.4MPa at most; the notched impact strength was only 31.1kJ/m2。
In patent application publication No. CN10931850A entitled "A discontinuous large linear length fiber reinforced thermoplastic composite material compression molded preform and method for making same", CFRTP continuous sheet material is cut into discontinuous sheet material with certain length and width and then pressed into preform, the impact strength is improved significantly, but the anisotropy is very obvious, the impact strength in different directions is about doubled, see Table 1 for details.
Table 1:
as can be seen from the above patent applications for non-continuous fiber-reinforced thermoplastic composites, there is currently no composite material having a tensile strength of more than 150MPa and a notched impact strength of more than 150kJ/m in all directions2The high strength, high impact discontinuous fiber reinforced thermoplastic of (1).
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform, and aims to solve the problems of insufficient strength and impact resistance and obvious anisotropy of a discontinuous fiber reinforced thermoplastic composite material.
Another object of the present invention is to provide a high-strength, high-impact-resistance discontinuous fiber-reinforced thermoplastic composite preform prepared by the above preparation method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform comprises the following steps:
(1) compounding thermoplastic resin, an auxiliary agent and continuous fibers into a continuous fiber reinforced thermoplastic sheet (CFRTP) with the thickness of 0.1-0.2 mm in a melting and dipping mode;
(2) cutting the continuous sheet into small sheets with the length and width of (10-50 mm) × (5-10 mm);
(3) Uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
(4) heating to melt the uniformly mixed small slices;
(5) then mixing the materials by low-shear mixing equipment to improve the uniformity of the materials;
(6) and cold-pressing the compound melt in the molten state into a sheet with a certain width and a thickness of 1-5 mm, wherein the sheet is the high-strength high-impact discontinuous fiber reinforced thermoplastic composite material preform.
In the step (1), the thermoplastic resin accounts for 28-65% by mass, the auxiliary agent accounts for 0.1-5% by mass, and the continuous fiber accounts for 30-70% by mass.
The thermoplastic resin in the step (1) comprises more than one of PE resin, PP resin, PA resin, PC resin, PMMA resin, PBT resin, PPS resin and the like.
The auxiliary agent in the step (1) comprises more than one of an antioxidant, a compatilizer, a lubricant and the like.
The continuous fiber in the step (1) comprises more than one of carbon fiber, glass fiber, aramid fiber and basalt fiber.
The melting impregnation in the step (1) is realized through a double-screw extruder, the thermoplastic resin and the auxiliary agent are uniformly mixed, and then the mixture is melted through the double-screw extruder and enters an impregnation die head to be melt impregnated with the continuous fibers.
The mixing in the step (3) is common mixing.
The heating in the step (4) is infrared heating or continuous oven heating.
The mixing time in the step (5) is 1-5 minutes.
The low-shear mixing device in the step (5) comprises a pin-type single-screw extruder or a low-shear twin-screw extruder, and the low-shear is generally referred to asShear rate of not higher than 102In seconds.
Compared with the prior art, the invention has the following advantages and effects:
compared with the existing preparation method, the discontinuous fiber reinforced thermoplastic composite material preform prepared by the invention has better uniformity, better isotropy and higher impact strength, and the notch impact strength in each direction exceeds 150kJ/m2。
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The invention relates to a preparation method of a high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite preform, which is suitable for thermoplastic plastics such as PE (polyethylene) resin, PP (polypropylene) resin, PA (polyamide) resin, PC (polycarbonate) resin, PBT (polybutylene terephthalate), PMMA (polymethyl methacrylate), PPS (polyphenylene sulfide) and the like, and comprises the following specific preparation steps of:
1. preparation of high-strength and high-impact-resistance discontinuous fiber reinforced PP composite material preform
Compounding PP resin, an auxiliary agent and continuous fibers (28-65 wt% of PP resin, 0.1-5 wt% of auxiliary agent and 30-70 wt% of continuous fibers) into a continuous fiber reinforced thermoplastic sheet (CFRTP) with the thickness of 0.1-0.2 mm in a melting impregnation mode, wherein the melting impregnation temperature is set to 230-280 ℃;
cutting the continuous sheet into small sheets with the length and width of (10-50 mm) × (5-10 mm);
uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
melting the small sheet material by infrared or other rapid heating modes;
fifthly, performing heat preservation mixing for 1-5 minutes by low-shear mixing equipment;
and sixthly, pressing the compound melt in the molten state into a sheet with a certain width and the thickness of 1-5mm by using a continuous double-belt press, wherein the temperature of the continuous double-belt press is set to be 175-200 ℃.
2. Preparation of high-strength and high-impact-resistance discontinuous fiber reinforced PA6 composite material preform
Compounding PA6 resin, an auxiliary agent and continuous fibers (28-65 wt% of PA6 resin, 0.1-5 wt% of auxiliary agent and 30-70 wt% of continuous fibers) into a continuous fiber reinforced thermoplastic sheet (CFRTP) with the thickness of 0.1-0.2 mm in a melt impregnation mode, wherein the melt impregnation temperature is set to be 260-320 ℃;
Cutting the continuous sheet into small sheets with the length and width of (10-50 mm) × (5-10 mm);
uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
melting the small sheet material by infrared or other rapid heating modes;
fifthly, performing heat preservation mixing for 1-5 minutes by low-shear mixing equipment;
sixthly, pressing the compound melt in the molten state into a sheet with a certain width and the thickness of 1-5mm by a continuous double-belt press, wherein the temperature of the continuous double-belt press is set to be 240-260 ℃.
3. Preparation of high-strength and high-impact-resistance discontinuous fiber reinforced PA66 composite material preform
Compounding PA66 resin, an auxiliary agent and continuous fibers (28-65 wt% of PA66 resin, 0.1-5 wt% of auxiliary agent and 30-70 wt% of continuous fibers) into a continuous fiber reinforced thermoplastic sheet (CFRTP) with the thickness of 0.1-0.2 mm in a melt impregnation mode, wherein the melt impregnation temperature is set to 270-330 ℃;
cutting the continuous sheet into small sheets with the length and width of (10-50 mm) × (5-10 mm);
uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
melting the small sheet material by infrared or other rapid heating modes;
Fifthly, performing heat preservation mixing for 1-5 minutes by low-shear mixing equipment;
sixthly, pressing the compound melt in the molten state into a sheet with a certain width and the thickness of 1-5mm by using a continuous double-belt press, wherein the temperature of the continuous double-belt press is set to be 270-290 ℃.
4. Preparation of high-strength and high-impact-resistance discontinuous fiber reinforced PC composite material preform
Compounding a PC resin, an auxiliary agent and continuous fibers (28-65 wt% of the PC resin, 0.1-5 wt% of the auxiliary agent and 30-70 wt% of the continuous fibers) into a continuous fiber reinforced thermoplastic sheet (CFRTP) with the thickness of 0.1-0.2 mm by a melt impregnation mode, wherein the melt impregnation temperature is set to be 300-330 ℃;
cutting the continuous sheet into small sheets with the length and width of (10-50 mm) × (5-10 mm);
uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
melting the small sheet material by infrared or other rapid heating modes;
fifthly, performing heat preservation mixing for 1-5 minutes by low-shear mixing equipment;
and sixthly, pressing the compound melt in the molten state into a sheet with a certain width and the thickness of 1-5mm by using a continuous double-belt press, wherein the temperature of the continuous double-belt press is set to be 270-300 ℃.
The specific implementation mode is as follows:
example 1
A high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform is prepared by the following steps:
(1) compounding PP resin, glass fiber, carbon fiber and an auxiliary agent (an antioxidant and a compatilizer) into a GF/PP prepreg sheet and a CF/PP continuous sheet with the thickness of 0.2mm in a melting and dipping mode; wherein the PP resin content is 38 wt%, the carbon fiber content is 40 wt%, the glass fiber content is 20 wt%, the antioxidant content is 0.2 wt%, and the compatilizer content is 1.8 wt%;
(2) cutting the continuous sheet into small sheets with the width of 5mm and the lengths of 10mm, 15mm, 35mm and 50 mm; wherein the ratio of the small sheets with the lengths of 10mm, 15mm, 35mm and 50mm is 1:2:3: 4;
(3) uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
(4) melting the uniformly mixed small slices by infrared rapid heating;
(5) then mixing for 1-5 minutes by low-shear mixing equipment to improve the uniformity of the material;
(6) the composite melt in the molten state was cold-pressed by a continuous double belt press into a sheet of 3mm thickness.
Comparative example 1
A discontinuous long fiber reinforced thermoplastic PP composite material preform is prepared by the following steps:
(1) Compounding PP resin, glass fiber, carbon fiber and an auxiliary agent (an antioxidant and a compatilizer) into a GF/PP prepreg sheet and a CF/PP continuous sheet with the thickness of 0.3mm in a melting and dipping mode; wherein the PP resin content is 38 wt%, the carbon fiber content is 40 wt%, the glass fiber content is 20 wt%, the antioxidant content is 0.2 wt%, and the compatilizer content is 1.8 wt%;
(2) cutting the continuous sheet into small sheets with the width of 5mm, the length of 10mm, 15mm, 35mm and 50 mm; wherein the ratio of the small sheets with the lengths of 10mm, 15mm, 35mm and 50mm is 1:2:3: 4;
(3) and mixing the small sheets, and then carrying out hot pressing to obtain a sheet with the thickness of 3 mm.
Example 2
A high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform is prepared by the following steps:
(1) compounding PP resin, glass fiber, carbon fiber and an auxiliary agent (an antioxidant and a compatilizer) into a GF/PP prepreg sheet and a CF/PP continuous sheet with the thickness of 0.2mm in a melting and dipping mode; wherein the PP resin content is 38 wt%, the carbon fiber content is 40 wt%, the glass fiber content is 20 wt%, the antioxidant content is 0.2 wt%, and the compatilizer content is 1.8 wt%;
(2) cutting the continuous sheet into small sheets with the width of 5mm, the length of 10mm, 15mm, 35mm and 50 mm; wherein the ratio of the small sheets with the lengths of 10mm, 15mm, 35mm and 50mm is 1:2:3: 4;
(3) Uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
(4) melting the uniformly mixed small slices by infrared rapid heating;
(5) then mixing for 1-5 minutes by low-shear mixing equipment to improve the uniformity of the material;
(6) the composite melt in the molten state was cold-pressed by a continuous double belt press into a sheet of 3mm thickness.
Comparative example 2
A discontinuous long fiber reinforced thermoplastic composite preform is prepared by the following steps:
(1) compounding PP resin, glass fiber, carbon fiber and an auxiliary agent (an antioxidant and a compatilizer) into a GF/PP prepreg sheet and a CF/PP continuous sheet with the thickness of 0.5mm in a melting and dipping mode; wherein the PP resin content is 38 wt%, the carbon fiber content is 40 wt%, the glass fiber content is 20 wt%, the antioxidant content is 0.2 wt%, and the compatilizer content is 1.8 wt%;
(2) cutting the continuous sheet into small sheets with the width of 5mm, the length of 10mm, 15mm, 35mm and 50 mm; wherein the ratio of the small sheets with the lengths of 10mm, 15mm, 35mm and 50mm is 1:2:3: 4;
(3) and mixing the small sheets, and then carrying out hot pressing to obtain a sheet with the thickness of 3 mm.
The sheet properties obtained in examples 1 to 2 and comparative examples 1 to 2 are shown in Table 2.
Table 2:
example 3
A high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform is prepared by the following steps:
(1) compounding PA6 resin, glass fiber and an auxiliary agent (antioxidant) into a continuous sheet with the thickness of 0.1mm in a melting and impregnating mode; wherein the content of the PA6 resin is 39.5 wt%, the content of the glass fiber is 60 wt%, and the content of the antioxidant is 0.5 wt%;
(2) cutting the continuous sheet into small sheets with the width of 5mm and the lengths of 10mm, 15mm, 35mm and 50 mm; wherein the ratio of the small sheets with the lengths of 10mm, 15mm, 35mm and 50mm is 1:2:3: 4;
(3) uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
(4) melting the uniformly mixed small slices by infrared rapid heating;
(5) then mixing for 1-5 minutes by low-shear mixing equipment to improve the uniformity of the material;
(6) the composite melt in the molten state was cold-pressed by a continuous double belt press into a sheet of 3mm thickness.
Comparative example 3
A discontinuous long fiber reinforced thermoplastic composite preform is prepared by the following steps:
(1) compounding PA6 resin, glass fiber and an auxiliary agent (antioxidant) into a continuous sheet with the thickness of 0.3mm in a melting and impregnating mode; wherein the content of the PA6 resin is 39.5 wt%, the content of the glass fiber is 60 wt%, and the content of the antioxidant is 0.5 wt%;
(2) Cutting the continuous sheet into small sheets with the width of 5mm, the length of 10mm, 15mm, 35mm and 50 mm; wherein the ratio of the small sheets with the lengths of 10mm, 15mm, 35mm and 50mm is 1:2:3: 4;
(3) and mixing the small sheets, and then carrying out hot pressing to obtain a sheet with the thickness of 3 mm.
Example 4
A high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform is prepared by the following steps:
(1) compounding PA6 resin, glass fiber and an auxiliary agent (antioxidant) into a continuous sheet with the thickness of 0.2mm in a melting and impregnating mode, wherein the glass fiber content is 60 wt%; wherein the content of the PA6 resin is 39.5 wt%, the content of the glass fiber is 60 wt%, and the content of the antioxidant is 0.5 wt%;
(2) cutting the continuous sheet into small sheets with the width of 5mm and the lengths of 10mm, 15mm, 35mm and 50 mm; wherein the ratio of the small sheets with the lengths of 10mm, 15mm, 35mm and 50mm is 1:2:3: 4;
(3) uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
(4) melting the uniformly mixed small slices by infrared rapid heating;
(5) then mixing for 1-5 minutes by low-shear mixing equipment to improve the uniformity of the material;
(6) the composite melt in the molten state was cold-pressed by a continuous double belt press into a sheet of 3mm thickness.
Comparative example 4
A discontinuous long fiber reinforced thermoplastic composite preform is prepared by the following steps:
(1) compounding PA6 resin, glass fiber and an auxiliary agent (antioxidant) into a continuous sheet with the thickness of 0.5mm in a melting and impregnating mode; wherein the content of the PA6 resin is 39.5 wt%, the content of the glass fiber is 60 wt%, and the content of the antioxidant is 0.5 wt%;
(2) cutting the continuous sheet into small sheets with the width of 5mm, the length of 10mm, 15mm, 35mm and 50 mm; wherein the ratio of the small sheets with the lengths of 10mm, 15mm, 35mm and 50mm is 1:2:3: 4;
(3) and mixing the small sheets, and then carrying out hot pressing to obtain a sheet with the thickness of 3 mm.
The sheet property test data obtained in examples 3 to 4 and comparative examples 3 to 4 are shown in Table 3.
Table 3:
the above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a high-strength and high-impact-resistance discontinuous fiber reinforced thermoplastic composite material preform is characterized by comprising the following steps:
(1) Compounding thermoplastic resin, an auxiliary agent and continuous fibers into a continuous fiber reinforced thermoplastic sheet with the thickness of 0.1-0.2 mm in a melting and dipping mode;
(2) cutting the continuous sheet into small sheets with the length and width of (10-50 mm) × (5-10 mm);
(3) uniformly mixing the cut small sheets to keep the isotropy of fiber distribution;
(4) heating to melt the uniformly mixed small slices;
(5) then mixing the materials by low-shear mixing equipment to improve the uniformity of the materials;
(6) and cold-pressing the compound melt in the molten state into a sheet with the thickness of 1-5 mm.
2. The preparation method of the high-strength high-impact discontinuous fiber reinforced thermoplastic composite preform according to claim 1, wherein in the step (1), the mass percentages of the thermoplastic plastic, the auxiliary agent and the continuous fiber are respectively 28-65%, 0.1-5% and 30-70%.
3. The method for preparing a high-strength high-impact discontinuous fiber-reinforced thermoplastic composite preform according to claim 1, wherein the thermoplastic resin in step (1) comprises one or more of PE resin, PP resin, PA resin, PC resin, PMMA resin, PBT resin and PPS resin.
4. The method for preparing a high-strength high-impact discontinuous fiber-reinforced thermoplastic composite preform according to claim 1, wherein the auxiliary agent in step (1) comprises one or more of an antioxidant, a lubricant and a compatilizer.
5. The method for preparing the high-strength high-impact discontinuous fiber reinforced thermoplastic composite preform according to claim 1, wherein the continuous fiber in the step (1) comprises more than one of carbon fiber, glass fiber, aramid fiber and basalt fiber.
6. The method for preparing a high-strength high-impact discontinuous fiber-reinforced thermoplastic composite preform according to claim 1, wherein the melt impregnation in the step (1) is performed by a twin-screw extruder, and the thermoplastic resin and the auxiliary agent are uniformly mixed, melted by the twin-screw extruder, and then fed into the impregnation die and the continuous fiber for melt impregnation.
7. The method for preparing a high-strength high-impact non-continuous fiber-reinforced thermoplastic composite preform according to claim 1, wherein the mixing in the step (3) is ordinary mixing.
8. The method for preparing a high-strength high-impact discontinuous fiber reinforced thermoplastic composite preform according to claim 1, wherein the heating in step (4) is infrared heating or continuous oven heating.
9. The method for preparing a high-strength high-impact non-continuous fiber-reinforced thermoplastic composite preform according to claim 1, wherein the low-shear mixing device of step (5) comprises a pin-type single-screw extruder or a low-shear twin-screw extruder, and the low-shear rate is not higher than 102In seconds.
10. A high-strength, high-impact non-continuous fiber-reinforced thermoplastic composite preform prepared by the method of any one of claims 1 to 9.
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