CN114605740B - Long glass fiber reinforced polypropylene material and preparation method and application thereof - Google Patents
Long glass fiber reinforced polypropylene material and preparation method and application thereof Download PDFInfo
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a long glass fiber reinforced polypropylene material, a preparation method and application thereof, wherein the material comprises the following components: polypropylene resin, polyamide resin, compatilizer, nylon elastomer, long glass fiber, aluminum powder and auxiliary agent. According to the invention, the uniform metal flickering effect is realized through the long glass fiber and the aluminum powder compounded with different particle diameters; aluminum powder is distributed on the surface of the workpiece and covers the floating fiber; long glass fibers are mutually interpenetrated, so that the material performance reduction caused by adding aluminum powder is avoided; and polyamide and nylon elastomer are added to improve scratch resistance and impact resistance. The material is suitable for the appearance structural member, is free from spraying, and has wide application prospect.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a long glass fiber reinforced polypropylene material and a preparation method and application thereof.
Background
The spraying-free material is used as an environment-friendly product, can avoid a spray painting link, and can enhance the competitiveness of the product under the double-carbon policy of carbon neutralization and carbon peak reaching.
CN201710383662 provides a spraying-free PP material with metallic luster, which comprises 90% -97% of PP, 1% -5% of aluminum silver strips, 0.2% -0.3% of antioxidant, 0.1% -0.2% of UV-resistant auxiliary agent, and 0.1% -0.5% of wax powder. The spraying-free PP material is prepared from aluminum silver strips with good dispersibility and a matrix resin PP material, and the prepared spraying-free PP material has high reflectivity, the aluminum silver strips (with the particle size of 30-35 mu m) are uniformly dispersed in the PP material, and the metallic luster is high.
CN102942742a provides a spray-free PP material with metallic sparkling effect, comprising 97% -99% of random PP, 0.2% -0.8% of antioxidant, 0.1% -1% of lubricant, 0.3% -1.5% of effect pigment. The spraying-free PP material can obtain good high-gloss and pearlescent flickering and metal paint spraying effects without spraying and direct injection molding, has good appearance, saves cost compared with a paint spraying process, and simultaneously avoids the paint stripping problem in the use process of the product.
CN106279971a discloses a spray-free highlight PP material, comprising 6% -9% of tetrahydrofuran, 0.1% -0.3% of tetraphenylphosphine palladium, 1% -2% of pearl powder, 1% -2% of toner, 0.3% -0.5% of lubricant, 0.3% -0.5% of nucleating agent, 0.3% -0.5% of liquid-shaped de-graining brightening agent, 0.5% -0.8% of liquid-shaped flow modifier, 0.3% -0.8% of liquid-shaped phase solvent, and the balance PP powder. The product has good surface highlight effect, uniform and continuous pearl powder layer is formed on the surface of the product, no flow lines exist, and the texture is strong.
The spraying-free polypropylene material belongs to a spraying-free material without a reinforcing system, and is characterized in that aluminum powder and glass fiber are easily sheared and crushed by the glass fiber in the double-screw melt blending process, so that the original surface metallic luster cannot be maintained. In addition, part of the metal powder or the pearl powder is easy to disperse unevenly, and accumulated in the resin system to cause uneven color of the product, and the metal powder or the pearl powder can reduce the tensile property and the toughness of the material. Meanwhile, the scratch-resistant effect of the system material is relatively poor.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide a long glass fiber reinforced polypropylene material, and a preparation method and application thereof. The material is free from spraying, has excellent metal effect, and simultaneously has good tensile property, scratch resistance and high toughness.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the long glass fiber reinforced polypropylene material comprises the following components in parts by weight: 12.8-78.2 parts of polypropylene resin, 5-20 parts of polyamide resin, 3-5 parts of compatilizer, 3-10 parts of nylon elastomer, 10-40 parts of long glass fiber, 0.2-5 parts of aluminum powder and 0-0.7 part of auxiliary agent.
Preferably, the long glass fiber reinforced polypropylene material comprises the following components in parts by weight: 28-70 parts of polypropylene resin, 10-15 parts of polyamide resin, 3-5 parts of compatilizer, 4-6 parts of nylon elastomer, 30-40 parts of long glass fiber, 2-4 parts of aluminum powder and 0.2-0.5 part of auxiliary agent.
Preferably, the polypropylene resin has a melt flow rate of 10-150g/10min (test conditions 230 ℃, 2.16kg, test standard ISO 1133). When the melt flow rate of the polypropylene resin is less than 10g/10min, the resin cannot fully impregnate the glass fiber, the impregnation die head has serious material returning or strip breakage, and smooth production cannot be realized.
Preferably, the polyamide resin is at least one of polyamide 6 (PA 6), polyamide 610 (PA 610), and polyamide 612 (PA 612).
Preferably, the compatibilizer is polypropylene grafted maleic anhydride (PP-G-MAH).
Preferably, the nylon elastomer is a copolymer composed of PA6 as a hard segment and propylene oxide polyether as a soft segment.
Preferably, the long glass fiber is twisted coarse sand, and the diameter of a monofilament is 7-18 mu m.
Preferably, the aluminum powder is a mixture of 55-100 μm particle size (D50) aluminum powder and 5-15 μm particle size aluminum powder; more preferably, the mass ratio (3-8) of the aluminum powder with the particle size of 55-100 μm to the aluminum powder with the particle size of 5-15 μm is as follows: 1.
Preferably, the auxiliary agent is at least one of an antioxidant and a lubricant.
The preparation method of the long glass fiber reinforced polypropylene material comprises the following steps: uniformly mixing polypropylene resin, polyamide resin, compatilizer, nylon elastomer, aluminum powder and auxiliary agent, melting, plasticizing and homogenizing at 275-330 ℃ and 400-800r/min to obtain resin auxiliary agent melt, and infiltrating long glass fiber at 320-350 ℃ to obtain the long glass fiber reinforced polypropylene material.
Preferably, the long glass fiber reinforced polypropylene material is cooled, shaped and granulated to obtain a finished product.
Preferably, the pellets are cut to a length of 6.+ -.3 mm or 10.+ -.3 mm.
Preferably, the melt plasticization homogenization is achieved using a twin screw extruder. Through the LFT pulling and extruding process, aluminum powder and glass fiber cannot be simultaneously generated in the double-screw extruder, and the problem that metal aluminum powder is excessively damaged by strong shearing of the glass fiber in the extruder to influence the metal effect is avoided.
Preferably, the infiltration is realized by adopting an infiltration die head, the resin auxiliary agent melt passes through the infiltration die head, and the long glass fiber is drawn by the drawing equipment to pass through the infiltration die head, so that the resin auxiliary agent melt infiltrates the long glass fiber.
Preferably, the speed of traction is 40-90m/min.
The long glass fiber reinforced polypropylene material is applied to the preparation of scratch-resistant and impact-resistant appearance structural members. The appearance structural member can be parts such as a lower guard plate, a foot support, an electric tool handle, a general joint, a door handle of an automobile, a rearview mirror bracket and the like.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the metal flickering effect of the material is realized through long glass fibers and aluminum powder compounded with different particle diameters: the large-particle-size aluminum powder is oriented along with the flow direction of the melt and part of the long glass fibers to provide a uniform metal effect, and the small-particle-size aluminum powder is inserted into the long glass fiber framework structure to provide a flickering metal point effect. Secondly, aluminum powder is distributed on the surface of the workpiece to play a role in covering floating fibers. Furthermore, long glass fibers are mutually inserted, a glass fiber three-dimensional framework structure in an injection molding part is provided, and material performance reduction caused by adding aluminum powder is avoided. The material can obtain gorgeous metal effect on the surface of the product by adopting a spraying-free process, thereby reducing the reject ratio of the product, reducing pollution, particularly carbon emission and reducing energy consumption. The surface hardness of the material is improved by adding polyamide, so that the scratch resistance of the composite material is provided. The nylon elastomer improves the impact resistance, particularly the low-temperature impact toughness, of the modified material. The material provided by the invention has excellent metal effect, good scratch resistance, good tensile property and high toughness.
Drawings
FIG. 1 is a diagram showing the effect of a long glass fiber reinforced polypropylene material product without flow marks and floating fibers.
FIG. 2 is a graph showing the effect of a long glass fiber reinforced polypropylene material product with severe flow marks and obvious fiber floats.
FIG. 3 is a graph showing the effect of a long glass fiber reinforced polypropylene material product with flow marks and no floating fibers.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples and the accompanying drawings.
In the examples, the experimental methods used are conventional methods unless otherwise specified, and the materials, reagents, etc. used, unless otherwise specified, are commercially available.
The following description of the raw materials used in the examples and comparative examples is provided, but is not limited to these materials:
polypropylene resin 1: molding, K9026; a melt flow rate of 26g/10min measured at a temperature of 230 ℃ using a weight of 2.16kg according to ISO 1133;
polypropylene resin 2: LG, MH7900; a melt flow rate of 150g/10min measured at a temperature of 230 ℃ using a weight of 2.16kg according to ISO 1133;
polypropylene resin 3: sea-pressing petrochemical PP PPH-T03; a melt flow rate of 4g/10min measured at a temperature of 230 ℃ using a weight of 2.16kg according to ISO 1133;
polyamide resin 1: PA6, sea-sun chemical fiber, HY2500A;
polyamide resin 2: PA610, shandong guang boundary new material limited, F120;
polyamide resin 3: PA612, shanghai curing company, inc, a150;
polypropylene grafted maleic anhydride: acarma, CA100;
nylon elastomer: atochem,5512MNOO; a copolymer composed of PA6 as a hard segment and propylene oxide polyether as a soft segment;
polyolefin elastomer: POE ENGAGE8137, dow;
long glass fiber: chongqing International composite material Co., ltd, ER4301R-2400; the diameter of each monofilament is 17 mu m;
short wave fiber: ECS301HP-3-H, chongqing International composite Material Co., ltd;
aluminum powder 1: the mass ratio of the compound fertilizer to the Xuanyang is (TH 5390) (particle size 85+/-2 mu m) to the XYC710 (particle size 10+/-2 mu m) is 3:1, compounding;
aluminum powder 2: the mass ratio of the compound fertilizer to the Xuanyang is (TH 5390) (particle size 85+/-2 mu m) to the XYC710 (particle size 10+/-2 mu m) is 2:1, compounding;
aluminum powder 3: the mass ratio of the compound fertilizer to the Xuanyang is (TH 5390) (particle size 85+/-2 mu m) to the XYC710 (particle size 10+/-2 mu m) is 9:1, compounding;
aluminum powder 4: the mass ratio of the compound fertilizer to the Xuanyang is (TH 5390) (particle size 85+/-2 mu m) to the XYC710 (particle size 10+/-2 mu m) is 8:1, compounding;
auxiliary agent: antioxidant, 1010, commercially available; a lubricant, erucamide, commercially available; the mass ratio of the antioxidant to the lubricant is 1:1.
examples 1 to 8 and comparative examples 1 to 12
The components and parts by weight of the long glass fiber reinforced polypropylene materials of examples 1 to 8 and comparative examples 1 to 12 are shown in tables 1 and 2. The preparation method of the polypropylene composite materials of examples 1-8 and comparative examples 1-12 comprises the following steps: the polypropylene resin, the polyamide resin, the compatilizer, the nylon elastomer aluminum powder and the auxiliary agent are uniformly mixed, and are fed into a double-screw extruder by a metering scale for melting plasticizing homogenization, wherein the temperature of the double-screw extruder is set to 290 ℃, and the rotating speed is 600r/min. The obtained resin auxiliary melt was fed to a infiltration die, the infiltration die temperature being set at 340 ℃. The long glass fiber is drawn by the drawing equipment and passes through the infiltration die head, the drawing speed is 50m/min, and the infiltration of the resin auxiliary agent melt to the long glass fiber is realized. The long glass fiber reinforced polypropylene material strip is obtained after the infiltration is completed, and then the long glass fiber reinforced polypropylene material strip is cooled, shaped and granulated to obtain a finished product with the length of 10 mm.
Table 1 raw material components and parts by weight in examples
Table 2 raw material components and parts by weight in comparative examples
Effect example Performance test
The long glass fiber reinforced polypropylene materials prepared in examples 1 to 8 and comparative examples 1 to 12 were subjected to the relevant performance test, and the specific test method is as follows:
the mechanical property test and evaluation method comprises the following steps: the tensile strength of the bars was tested according to ISO527-1/2 standard at 23 ℃; the bars were tested for notched impact strength at 23℃according to ISO179/1eA standard.
The low-temperature ball drop impact performance test and evaluation method comprises the following steps: the material is subjected to injection molding to form a square plate with the thickness of 2mm, the material is stored for 24 hours at the temperature of minus 40 ℃, 500g of iron balls and 40mm of falling balls are used for falling impact, and whether cracks exist or not is observed.
The metal effect evaluation method comprises the following steps: observing whether the metal effect is uniform, whether the flicker effect is obvious, and whether the metal effect has flow marks and floating fiber defects: the more uniform the metal effect, the more pronounced the sparkling effect, the better the spray effect, expressed as visual effect, the more representative the better the effect.
The scratch resistance effect evaluation method comprises the following steps: scratch resistance delta L values were tested for 15N force scratch according to the PV3952 standard.
The floating fiber and flow mark rating method comprises the following steps: visual inspection. The state without floating fiber and without flow mark is shown in fig. 1, the state with serious flow mark and obvious floating fiber is shown in fig. 2, and the state without floating fiber and with flow mark is shown in fig. 3.
Table 3 results of performance testing of examples
Table 4 results of Performance test of comparative examples
The invention adds polyamide and nylon elastomer to improve the scratch resistance and impact resistance of the modified material, especially the low-temperature impact toughness. Aluminum powder with proper proportion is added, so that the impact strength, the metal flickering effect and the metal uniformity effect of the material are improved, and the product has no flow mark and floating fiber. The material provided by the invention has excellent metal effect, tensile property, scratch resistance and high toughness. Fig. 1 is a graph showing the effect of the long glass fiber reinforced polypropylene material of example 3, and it can be seen that the material exhibits a uniform metal effect, has a flickering metal point effect, well covers floating fibers, and has no flow mark. Examples 1, 2 and 7 used less long glass fibers, but the tensile strength and notched impact strength at room temperature still reached relatively high levels.
The data in table 4 can be seen: comparative example 1, short glass fiber has poor toughness, very poor metal effect, severe flow marks and obvious fiber floating; comparative example 2: no polyamide exists, the metal effect is good, but the toughness is poor, the appearance is poor, and the scratch resistance effect is poor; comparative example 3: no aluminum powder is added, and the metal effect cannot be realized; comparative example 4: nylon elastomer is not used, and the toughness is poor; comparative example 5: the aluminum powder is too little in dosage, the metal effect is poor, flow marks are formed, and the flicker effect is poor; comparative example 6: excessive aluminum powder is used, has flow marks and has poor flickering effect; comparative example 7: the aluminum powder with small particle size has overlarge proportion, poor metal uniformity effect and flow marks; comparative example 8: the aluminum powder with large particle size has over large proportion, poor flicker effect and flow marks; comparative example 9: the glass fiber can not be fully impregnated by the resin, the material returning or strip breakage of the impregnation die head is serious, and the smooth production can not be realized; comparative example 10: poor metal effect and flicker effect, poor impact strength of falling balls at low temperature; comparative example 11: poor metal effect and flicker effect, poor impact strength of falling balls at low temperature, and floating fiber; comparative example 12: the polyolefin elastomer has poor metal effect and flicker effect, and poor impact strength of falling balls at low temperature.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. The long glass fiber reinforced polypropylene material is characterized by comprising the following components in parts by weight: 12.8-78.2 parts of polypropylene resin, 5-20 parts of polyamide resin, 3-5 parts of compatilizer, 4-6 parts of nylon elastomer, 10-40 parts of long glass fiber, 2-4 parts of aluminum powder and 0-0.7 part of auxiliary agent;
the melt flow rate of the polypropylene resin under the test condition of 2.16kg at 230 ℃ is 10-150g/10min;
the aluminum powder is a mixture of 55-100 mu m grain size aluminum powder and 5-15 mu m grain size aluminum powder, and the mass ratio of the 55-100 mu m grain size aluminum powder to the 5-15 mu m grain size aluminum powder is (3-8): 1.
2. The long glass fiber reinforced polypropylene material according to claim 1, wherein the long glass fiber reinforced polypropylene material comprises the following components in parts by weight: 28-70 parts of polypropylene resin, 10-15 parts of polyamide resin, 3-5 parts of compatilizer, 4-6 parts of nylon elastomer, 30-40 parts of long glass fiber, 2-4 parts of aluminum powder and 0.2-0.5 part of auxiliary agent.
3. The long glass fiber reinforced polypropylene material according to claim 1, wherein,
the polyamide resin is at least one of PA6, PA610 and PA 612;
the compatilizer is polypropylene grafted maleic anhydride;
the nylon elastomer is a copolymer which takes PA6 as a hard segment and propylene oxide polyether as a soft segment.
4. The long glass fiber reinforced polypropylene material according to claim 1, wherein the long glass fiber is twisted coarse sand, and the diameter of the monofilament is 7-18 μm 。
5. The long glass fiber reinforced polypropylene material according to claim 1, wherein the auxiliary agent is at least one of an antioxidant and a lubricant.
6. The method for preparing the long glass fiber reinforced polypropylene material according to any one of claims 1 to 5, comprising the following steps: uniformly mixing polypropylene resin, polyamide resin, compatilizer, nylon elastomer, aluminum powder and auxiliary agent, and melting, plasticizing and homogenizing at 275-330 ℃ and 400-800r/min to obtain resin auxiliary agent melt, and infiltrating long glass fiber at 320-350 ℃ to obtain a long glass fiber reinforced polypropylene material;
the long glass fiber reinforced polypropylene material is cooled, shaped and granulated to obtain a finished product;
the melting plasticizing homogenization is realized by a double-screw extruder;
the infiltration is realized by adopting an infiltration die head.
7. Use of the long glass fiber reinforced polypropylene material according to any one of claims 1 to 5 for the preparation of scratch-resistant and impact-resistant appearance structural members.
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| CN202210321085.8A CN114605740B (en) | 2022-03-29 | 2022-03-29 | Long glass fiber reinforced polypropylene material and preparation method and application thereof |
| PCT/CN2023/082077 WO2023185504A1 (en) | 2022-03-29 | 2023-03-17 | Long glass fiber reinforced polypropylene material and preparation method therefor and application thereof |
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| CN115449157B (en) * | 2022-09-30 | 2023-12-19 | 江苏金发科技新材料有限公司 | Long glass fiber reinforced polypropylene material and preparation method and application thereof |
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| JP6946653B2 (en) * | 2017-02-03 | 2021-10-06 | トヨタ紡織株式会社 | Fiber reinforced materials and structures |
| CN108047627A (en) * | 2017-12-25 | 2018-05-18 | 会通新材料股份有限公司 | It is a kind of to exempt from spray coating polypropylene composite material and preparation method thereof with scratch resistant, metallic silver texture |
| KR102153795B1 (en) * | 2018-10-05 | 2020-09-08 | 한화토탈 주식회사 | Highly rigid composite resin composition with excellent feeling to touch and heat resistance and article molded therefrom |
| CN114605740B (en) * | 2022-03-29 | 2023-10-03 | 江苏金发科技新材料有限公司 | Long glass fiber reinforced polypropylene material and preparation method and application thereof |
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| CA2606611A1 (en) * | 2005-05-17 | 2006-11-23 | Exxonmobil Research And Engineering Company | Cloth-like fiber reinforced polypropylene compositions and method of making thereof |
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| CN111363248A (en) * | 2020-05-07 | 2020-07-03 | 苏州禾润昌新材料有限公司 | Spraying-free polypropylene composite material for automobile bumper decoration strip and preparation method thereof |
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| WO2023185504A1 (en) | 2023-10-05 |
| CN114605740A (en) | 2022-06-10 |
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