CN108690347B - Carbon fiber reinforced nylon composite material and preparation method thereof - Google Patents

Carbon fiber reinforced nylon composite material and preparation method thereof Download PDF

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CN108690347B
CN108690347B CN201710229515.2A CN201710229515A CN108690347B CN 108690347 B CN108690347 B CN 108690347B CN 201710229515 A CN201710229515 A CN 201710229515A CN 108690347 B CN108690347 B CN 108690347B
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carbon fiber
composite material
fiber reinforced
reinforced nylon
nylon composite
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CN108690347A (en
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黄险波
陈大华
范欣愉
蒲颖
孙雅杰
李晓拓
刘玲
宋威
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Guangzhou Kingfa Carbon Fiber New Material Development Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/04Ingredients characterised by their shape and organic or inorganic ingredients
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/042Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with carbon fibres
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
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    • C08K5/20Carboxylic acid amides
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2377/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/004Additives being defined by their length

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Abstract

The invention discloses a carbon fiber reinforced nylon composite material and a preparation method thereof. The carbon fiber reinforced nylon composite material comprises the following components in percentage by weight: 50% -75% of nylon resin; 0% -10% of an auxiliary agent; 20% -40% of carbon fibers; in the carbon fiber reinforced nylon composite material, the retention length and the distribution of carbon fibers comprise the following components in percentage by weight: less than 1200um 15% -25%; 65% -75% of 1200 um-1800 um; more than 1800um 5% -10%. The prepared carbon fiber reinforced nylon composite material has excellent shock resistance while enhancing rigidity, achieves rigidity balance, and increases the applicability and practicability of nylon materials.

Description

Carbon fiber reinforced nylon composite material and preparation method thereof
Technical Field
The invention relates to the technical field of thermoplastic composite materials, in particular to a carbon fiber reinforced nylon composite material.
Background
Carbon Fiber (CF) is a new fiber material of high-strength and high-modulus fiber with carbon content above 95%. It is made up by stacking organic fibres of flake graphite microcrystals along the axial direction of fibre, and making carbonization and graphitization treatment so as to obtain the invented microcrystal graphite material. The carbon fiber is flexible outside and rigid inside, has lighter weight than metal aluminum, higher strength than steel, corrosion resistance and high modulus, and is an important material in national defense, military industry and civil use. It not only has the intrinsic characteristic of carbon material, but also has the soft workability of textile fiber, and is a new generation of reinforced fiber.
The carbon fiber reinforced thermoplastic (resin-based) composite material (LCFT) has the outstanding characteristics of light weight, high performance, high production efficiency, easiness in recovery, recyclability and the like, has obvious recoverability advantage compared with a thermosetting (resin-based) composite material (LCFP), and can be manufactured by adopting high-efficiency processes such as injection molding, mold pressing and the like. The carbon fiber is a high-modulus and high-strength material, the rigidity of the material can be greatly improved by adding the carbon fiber, but the impact resistance of the material is reduced due to the increase of the rigidity of the material, and the rigidity balance cannot be achieved. Therefore, a technological solution is urgently needed, so that the composite material has excellent impact resistance while the rigidity is enhanced, the rigidity and toughness balance is achieved, and the applicability and practicability of the material are improved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the carbon fiber reinforced nylon composite material to achieve rigidity and toughness balance.
The invention also aims to provide a preparation method of the carbon fiber reinforced nylon composite material.
The above object of the present invention is achieved by the following technical solutions:
The carbon fiber reinforced nylon composite material comprises the following components in percentage by weight:
50% -75% of nylon resin;
0% -10% of an auxiliary agent;
20% -40% of carbon fibers;
the carbon fiber retention length and the distribution thereof in the carbon fiber reinforced nylon composite material are calculated according to the weight percentage, and the carbon fiber retention length comprises the following components:
less than 1200um 15% -25%;
1200um~1800um 65%~75%;
more than 1800um 5% -10%.
The inventor finds that the carbon fiber reinforced nylon composite material comprises the following components in percentage by weight by adjusting the retention length and the content distribution of carbon fibers and realizing the retention length and the distribution of the carbon fibers: less than 1200um 15% -25%; 1200 um-1800 um 65% -75%; more than 1800um 5% -10%. The obtained carbon fiber reinforced nylon composite material has excellent toughness while enhancing the rigidity, achieves rigidity-toughness balance, and increases the applicability and practicability of the material.
Preferably, the carbon fiber retention length and the distribution thereof comprise the following components in percentage by weight:
less than 1200um 15% -20%;
1200um~1800um 70%~75%;
more than 1800um 7% -10%.
The nylon resin is one or more of PA6, PA66 and PA 610.
Preferably, the nylon resin is PA 6.
Preferably, the number average molecular weight of the PA6 is 13000-23000.
The auxiliary agent is a common auxiliary agent in the prior art, and mainly comprises one or more of an antioxidant, a lubricant, a compatilizer, a nucleating agent and a weather-resistant agent, such as an antioxidant 1010, Nauguard 445, a lubricant TAF, paraffin, a compatilizer Bondyram1001, a nucleating agent talcum powder, mica, a weather-resistant agent hindered amine and the like.
The diameter of the carbon fiber is 5um ~7 um.
The preparation method of the carbon fiber reinforced nylon composite material comprises the following steps:
s1, uniformly mixing nylon resin and an auxiliary agent, adding the mixture into a double-screw extruder, connecting an impregnation device at a die head of the extruder, wherein the temperature of the extruder is 200-260 ℃, and the temperature of the die head is 260-280 ℃;
s2, plasticizing through a double-screw extruder, conveying the high-temperature mixture melt to a die head, conveying the carbon fibers to the die head through a traction device, and forcedly dipping;
s3, pulling out the fully impregnated carbon fibers, cooling, shaping, and granulating to obtain particles with the length of 6-25 mm;
s4, putting the particles into an injection molding machine, and setting injection molding process parameters to prepare the carbon fiber reinforced nylon composite material;
the injection molding process parameters of the step S4 include: the injection pressure is 80-90 MPa, the backpressure pressure is 30-40 MPa, the screw rotating speed is 30-40 rpm, the injection speed is 60-70 mm/s, and the injection molding temperature is 280-290 ℃.
The test method of the retention length and distribution of the carbon fiber comprises the following steps: burning 2g of carbon fiber reinforced nylon composite material product at 600 ℃ in concentrated sulfuric acid and hydrofluoric acid, adjusting to neutrality through hydrogen peroxide titration, obtaining clear and transparent burning solution, cooling the liquid to room temperature, transferring 2ml of the liquid to a clean glass sheet from the bottom through a pipette, spreading the liquid drop into a water layer with the thickness of 2mm, taking a picture under the condition that the magnification of a secondary imaging instrument is 200 times, and calculating the retention length and distribution of carbon fibers by a statistical method according to the carbon fiber morphology of the picture.
Compared with the prior art, the invention has the following beneficial effects:
the carbon fiber retention length and the distribution thereof in the carbon fiber reinforced nylon composite material provided by the invention comprise the following components in percentage by weight: less than 1200um 15% -25%; 1200 um-1800 um 65% -75%; more than 1800um 5% -10%. Finally, the high rigidity of the nylon material is ensured, the shock resistance of the nylon material is obviously improved, and the applicability and the practicability of the material are greatly improved.
Detailed Description
The present invention is further explained with reference to specific embodiments, which are described in detail and specific, but not to be construed as limiting the scope of the invention, the technical solutions obtained by equivalents or equivalent changes should be included in the scope of the claims of the present invention.
The mechanical property testing method comprises the following steps:
tensile strength: ISO 527;
bending strength: ISO 178;
izod notched impact strength: ISO 180/1 a.
The raw materials adopted in the invention are as follows:
nylon resin: PA6, 1010C2 Mitsubishi, number average molecular weight 22000;
antioxidant: nauguard 445;
lubricant: TAF suzhongthailand photochemical assistant, ltd;
carbon fiber: t700, diameter 7um;
examples 1 to 8 and comparative examples 1 to 10
Preparing a carbon fiber reinforced nylon composite material:
s1, uniformly mixing nylon resin and an auxiliary agent, adding the mixture into a double-screw extruder, connecting an impregnation device at a die head of the extruder, wherein the temperature of the extruder is 200-260 ℃, and the temperature of the die head is 260-280 ℃;
s2, plasticizing through a double-screw extruder, conveying the high-temperature mixture melt to a die head, conveying the carbon fibers to the die head through a traction device, and forcedly dipping;
s3, pulling out the fully impregnated carbon fibers, cooling, shaping, and granulating to obtain particles with the length of 6-25 mm;
s4, putting the particles into an injection molding machine, and setting injection molding process parameters to prepare the carbon fiber reinforced nylon composite material; the injection molding process parameters are shown in table 1.
TABLE 1 specific formulations (in weight percent) of examples 1-8 and comparative examples 1-10 and their test performance results
Figure DEST_PATH_IMAGE001
TABLE 1
Figure 235143DEST_PATH_IMAGE002
As can be seen from the comparison of the data in Table 1, the retained length and distribution of the carbon fibers in the products obtained in examples 1-8 are calculated according to the weight percentage, and the retained length and distribution of the carbon fibers comprise less than 1200um 15% -25%; 1200 um-1800 um 65% -75%; more than 1800um 5% -10%. The retention length and distribution of the carbon fibers in the products obtained in the comparative examples 1 to 10 do not accord with the component distribution condition. The carbon fiber reinforced nylon composite material prepared in the embodiment not only obviously improves the impact resistance of the material, but also improves the tensile bending strength to a certain extent. The impact resistance of the material is ensured under the condition of improving the rigidity of the material, and the applicability and the practicability of the material are improved.

Claims (9)

1. The carbon fiber reinforced nylon composite material is characterized by comprising the following components in percentage by weight:
50% -75% of nylon resin;
0 to 10 percent of auxiliary agent;
20% -40% of carbon fiber;
the carbon fiber reinforced nylon composite material comprises the following components in percentage by weight according to the remaining length and distribution of carbon fibers:
less than 1200 μm 15% -25%;
1200μm~1800μm 65%~75%;
5 to 10 percent of grain with the diameter of more than 1800 mu m.
2. The carbon fiber reinforced nylon composite material as claimed in claim 1, wherein the carbon fiber retention length and the distribution thereof comprise the following components by weight percent:
Less than 1200 μm 15% -20%;
1200μm~1800μm 70%~75%;
7 to 10 percent of more than 1800 mu m.
3. The carbon fiber reinforced nylon composite material according to claim 1, wherein the nylon resin is one or more of PA6, PA66 and PA 610.
4. The carbon fiber reinforced nylon composite material according to claim 3, wherein the nylon resin is PA 6.
5. The carbon fiber reinforced nylon composite material as claimed in claim 4, wherein the PA6 has a number average molecular weight of 13000-23000.
6. The carbon fiber reinforced nylon composite material of claim 1, wherein the auxiliary agent is one or more of an antioxidant, a lubricant, a compatilizer, a nucleating agent and a weather-resistant agent.
7. The carbon fiber reinforced nylon composite material according to claim 1, wherein the carbon fiber has a diameter of 5 to 7 μm.
8. The method for preparing the carbon fiber reinforced nylon composite material as claimed in claim 1, which comprises the following steps:
s1, uniformly mixing nylon resin and an auxiliary agent, adding the mixture into a double-screw extruder, connecting an impregnation device at a die head of the extruder, wherein the temperature of the extruder is 200-260 ℃, and the temperature of the die head is 260-280 ℃;
S2, plasticizing through a double-screw extruder, conveying the high-temperature mixture melt to a die head, conveying the carbon fibers to the die head through a traction device, and forcedly dipping;
s3, pulling out the fully impregnated carbon fibers, cooling, shaping, and granulating to obtain particles with the length of 6-25 mm;
s4, putting the particles into an injection molding machine, and setting injection molding process parameters to prepare the carbon fiber reinforced nylon composite material;
the injection molding process parameters of the step S4 include: the injection pressure is 80-90 MPa, the backpressure pressure is 30-40 MPa, the screw rotation speed is 30-40 rpm, the injection speed is 60-70 mm/s, and the injection temperature is 280-290 ℃.
9. The carbon fiber reinforced nylon composite material of claim 1, wherein the test method of the carbon fiber retention length and the distribution thereof is as follows: burning 2g of carbon fiber reinforced nylon composite material product at 600 ℃ in concentrated sulfuric acid and hydrofluoric acid, titrating with hydrogen peroxide to be neutral to obtain a clear and transparent burning solution, cooling the liquid to room temperature, transferring 2ml of the liquid to a clean glass sheet from the bottom through a transfer pipette, spreading liquid drops to form a water layer with the thickness of 2mm, taking a picture under the condition that the magnification of a secondary imaging instrument is 200 times, and calculating the retention length and distribution of carbon fibers by a statistical method according to the carbon fiber morphology of the picture.
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CN109852045B (en) * 2018-12-24 2022-03-25 余姚中国塑料城塑料研究院 Microporous foamed long carbon fiber reinforced PA11 material and preparation method thereof
CN110760183A (en) * 2019-09-16 2020-02-07 安徽旭升新材料有限公司 Preparation method of PA66 carbon fiber composite material
CN113968059A (en) * 2021-12-04 2022-01-25 宁波瑞成包装材料有限公司 Production method of toughened BOPA film

Citations (2)

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US6066395A (en) * 1997-05-23 2000-05-23 Toray Industries, Inc. Chopped carbon fibers and a production process there of
CN105131547A (en) * 2015-08-28 2015-12-09 金发科技股份有限公司 Polycarbonate composition and preparing method thereof

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US7026388B2 (en) * 2001-03-28 2006-04-11 Ube Industries, Ltd. Conductive resin composition and process for producing the same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6066395A (en) * 1997-05-23 2000-05-23 Toray Industries, Inc. Chopped carbon fibers and a production process there of
CN105131547A (en) * 2015-08-28 2015-12-09 金发科技股份有限公司 Polycarbonate composition and preparing method thereof

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