CN114621521A - Long fiber reinforced polypropylene material and preparation method and application thereof - Google Patents
Long fiber reinforced polypropylene material and preparation method and application thereof Download PDFInfo
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- CN114621521A CN114621521A CN202210288697.1A CN202210288697A CN114621521A CN 114621521 A CN114621521 A CN 114621521A CN 202210288697 A CN202210288697 A CN 202210288697A CN 114621521 A CN114621521 A CN 114621521A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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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- C—CHEMISTRY; METALLURGY
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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Abstract
The invention discloses a long fiber reinforced polypropylene material and a preparation method and application thereof, wherein the long fiber reinforced polypropylene material comprises the following components in parts by weight: 29-70 parts of polypropylene, 3-10 parts of ultrahigh molecular weight polyethylene, 3-15 parts of polyvinyl butyral, 3-8 parts of maleic anhydride grafted POE, 20-50 parts of long glass fiber and 0.3-1.2 parts of wollastonite. The long fiber reinforced polypropylene material provided by the invention has smooth and good surface appearance, high tensile strength and notch impact strength, excellent toughness and good extrusion performance, and is suitable for extrusion molding process.
Description
Technical Field
The invention relates to the technical field of macromolecules, in particular to a long fiber reinforced polypropylene material and a preparation method and application thereof.
Background
The LFT material (long fiber reinforced thermoplastic material) is widely applied to the fields of automobile parts such as a front end frame, a fan bracket, an instrument panel framework, a 5G antenna housing, an industrial fan, an electric tool and the like due to the advantages of high strength, high rigidity and the like, the parts are mainly formed by injection molding, but the LFT material has poor toughness, and the use of the LFT material in the environments of impact resistance and drop resistance is limited. In addition, the LFT material is rarely reported in the field of extrusion molding process, mainly because: when the LFT material is subjected to an extrusion process, the plane of a workpiece is easy to collapse, and continuous production cannot be realized; the surface has serious fiber floating, and long fibers are easy to puncture the surface of a workpiece; and the extruded part is easy to deform. Therefore, how to develop an LFT material suitable for extrusion molding, improve the toughness of the material, and be suitable for working conditions of drop and impact resistance is a problem to be solved urgently.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a long fiber reinforced polypropylene material and a preparation method thereof. The long fiber reinforced polypropylene material provided by the invention has good toughness and appearance, and is very suitable for preparing materials in an extrusion molding process.
The method is realized by the following technical scheme:
the long fiber reinforced polypropylene material comprises the following components in parts by weight:
preferably, the composition comprises the following components in parts by weight:
further, the length-diameter ratio of the wollastonite is (13-20): 1, the length-diameter ratio of the wollastonite is (15-18): 1. wollastonite can improve the stiffness in the melt extrusion process and reduce the collapse phenomenon. However, the length to diameter ratio of wollastonite affects "stiffness". In the extrusion process, wollastonite is oriented along with the flow direction of the melt, so that the rigidity of the flow direction is provided, the melt strength is enhanced, and the stiffness of the extruded profile is improved. The length-diameter ratio is too small, the reinforcing effect of the wollastonite is not obvious, and the length-diameter ratio is too large, so that the wollastonite is not easy to orient along the melt flowing direction, and the phenomenon of broken bars is easily caused.
The addition of the polyvinyl butyral can improve the film forming property of the material in a laminar flow area close to the die head and reduce the roughness of the surface of a workpiece; and the binding force between the material and the glass fiber can be improved, so that the long glass fiber which is punctured outwards can be effectively wrapped by the long fiber reinforced polypropylene material in the extrusion and expansion process, the fiber floating phenomenon of a workpiece is reduced, and the smooth appearance of the surface of the workpiece is ensured. In addition, the addition of polyvinyl butyral and maleic anhydride grafted POE can also improve the toughness of the material.
Further, the ethylene content of the polypropylene is more than 18 wt%, preferably the ethylene content of the polypropylene is 21-24 wt%. When the ethylene content of the polypropylene is less than or equal to 18 wt%, the impact toughness of the polypropylene is low; when the ethylene content in the polypropylene is 21-24 wt%, the toughness of the material is good, the material is cooled slowly, enough time is provided for covering the long glass fibers, the number of the outwardly-penetrated long glass fibers can be reduced, and the appearance of the final material is better.
Further, the molecular weight of the ultra-high molecular weight polyethylene is more than 150 ten thousand. The ultrahigh molecular weight polyethylene is pultruded into a continuous fiber structure in the extrusion process, is inserted between the glass fiber and the resin and is oriented along the radial direction of an extruded part, plays a role in reinforcing a framework, particularly can improve the melt strength of a middle turbulent flow zone, and realizes efficient continuous production. The molecular weight of the selected ultra-high molecular weight polyethylene is more than 150 ten thousand, which is beneficial to enhancing the melt strength and helping to solve the problem of surface collapse.
Further, 0.6-2 parts of an auxiliary agent is also included. The auxiliary agent is one or two of an antioxidant or a lubricant.
The antioxidant is organic phosphite ester, alkylated monophenol or polyhydric phenol, an alkylation reaction product of polyhydric phenol and diene, a butylated reaction product of p-cresol or dicyclopentadiene, alkylated hydroquinones, hydroxylated thiodiphenyl ethers, alkylene-bisphenol, benzyl compounds or polyol esters, preferably, the antioxidant is one or more of antioxidant 412S, antioxidant 1010, antioxidant 1076 and antioxidant 168.
The lubricant may be a fatty acid based lubricant selected from one or more of a fatty acid, a fatty acid derivative or a fatty acid ester.
The invention also provides a preparation method of the long fiber reinforced polypropylene material, which comprises the following steps:
s1, weighing the components according to the proportion, premixing the components except for the long glass fiber, putting the components into an extruder for melting plasticization and homogenization to form a melt, and finally conveying the melt to an impregnation die head;
s2: the traction equipment pulls the long glass fiber to pass through the impregnation die head, so that the continuous glass fiber is impregnated by the melt;
s3: and cooling, shaping and granulating the material strips obtained after the impregnation is finished to obtain the long fiber reinforced polypropylene material.
Further, the extruder is a twin-screw extruder, the temperature of the twin-screw extruder is 275-330 ℃, the screw rotation speed of the twin-screw extruder is 400-800r/min, and the temperature of the impregnation die head in the step S1 is 320-350 ℃.
Further, in the step S2, the drawing speed of the drawing equipment is 40-90m/min, and the material is cut into 6 plus or minus 3mm or 10 plus or minus 3mm in length during cutting.
The invention also provides application of the long fiber reinforced polypropylene material in extrusion molding design products, such as automobile air filter air inlet pipes, active air inlet grille blades, office table decorative strips and the like.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a long fiber reinforced polypropylene material, and polyvinyl butyral is used for reducing floating fibers and ensuring the appearance smoothness of the surface of a product. The ultrahigh molecular weight polyethylene is pultruded into a continuous fiber structure in the extrusion process, the continuous fiber structure plays a role of reinforcing a framework, the melt strength of the intermediate turbulent flow zone is improved, the degree of surface collapse is reduced, and efficient continuous production is realized. The wollastonite further improves the stiffness in the melt extrusion process and reduces the collapse phenomenon. And polyvinyl butyral and maleic anhydride grafted POE can improve the toughness of the material and the toughness of the product. In addition, the long fiber reinforced polypropylene material provided by the invention has high extrusion efficiency and can be suitable for extrusion molding.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
< production of examples and comparative examples >
The raw materials used in the examples and comparative examples of the present invention include, but are not limited to, the following:
polypropylene:
polypropylene A: ethylene content of about 19%, grade PP 7033N, available from Exxon Mobil;
polypropylene B: ethylene content of about 10%, brand BX3800, available from SK, korea;
polypropylene C: ethylene content was about 21%, and the trade name EP548RQ, available from Tianjin Zhongsha.
Polypropylene D: ethylene content 24%, designation PP SP179, purchased from yanshan petrochemical.
In the invention, the content of ethylene in polypropylene is measured by infrared spectroscopy.
Ultra-high molecular weight polyethylene a: molecular weight 750 ten thousand, designation UH981, available from asahi chemical;
ultra-high molecular weight polyethylene B: molecular weight 100 ten thousand, designation 145M, purchased from mitsui chemistry;
polyvinyl butyral: brand TB-2, purchased from aerospace vehicle;
maleic anhydride grafted POE: the grafting yield was 0.5%, designation N493, purchased from dow chemical;
long glass fibers: the trade name ER4301R-2400, purchased from Chongqing International composite Co., Ltd;
wollastonite A: the length-diameter ratio is 13: 1, No. XYNFW-F50, available from southern wollastonite, Inc., New York;
wollastonite B: the length-diameter ratio is 15: 1, No. XYNFW-F55, available from southern wollastonite, Inc., New York;
wollastonite C: the length-diameter ratio is 18: 1, trade designation XYNFW-F60, purchased from southern wollastonite, ltd, new yu city;
wollastonite D: the length-diameter ratio is 20: 1, No. XYNFW-F65, available from southern wollastonite, Inc., New York;
wollastonite E: the length-diameter ratio is 3: 1, trade name XYNFW-SA, purchased from southern wollastonite, Inc., of Xinyu city;
wollastonite F: aspect ratio 25: 1, No. XYNFW-F70, available from southern wollastonite, Inc., New York;
antioxidant: commercially available, and used in the examples and comparative examples are the same species;
lubricant: erucamide, commercially available, and used in the examples and comparative examples is the same material.
The preparation methods of the examples and comparative examples of the present invention are as follows:
s1, weighing the components according to the proportion, premixing the components except the long glass fiber, putting the components into an extruder for melting plasticization and homogenization to form a melt, and finally conveying the melt to an impregnation die head;
s2: the traction equipment pulls the long glass fiber to pass through the impregnation die head, so that the continuous glass fiber is impregnated by the melt;
s3: and cooling, shaping and granulating the material strips obtained after the impregnation is finished to obtain the long fiber reinforced polypropylene material.
The extruder is a double-screw extruder, the temperature of the double-screw extruder is 275-330 ℃, the screw rotating speed of the double-screw extruder is 500r/min, and the temperature of the impregnation die head in the step S1 is 320-350 ℃.
In step S2, the pulling speed of the pulling device is 50 m/min.
In the present specification, the term "part(s)" means "part(s) by weight" unless otherwise specified.
< test standards >
The performance test standards of the examples of the present invention and the comparative examples are as follows:
tensile strength: at 23 ℃ according to ISO 527-2: 2012 standard test bars for tensile strength;
notched impact strength: at 23 ℃ according to ISO 179-1: 2010 testing the notch impact strength of the sample strip;
impact of falling ball: according to the standard PV3905, a 2mm square plate is subjected to material injection molding, 500g of iron balls are used, 40mm falling balls are subjected to falling impact, and whether cracks exist is observed;
extrusion performance:
(1) in the extrusion process, the rotating speed of the extruder is fixed at 200 r/min and the temperature is fixed at 180 ℃, the time from the die head of the extruder to the natural falling of the melt to the ground is recorded as T, and the higher the T, the higher the melt strength is.
(2) In the extrusion process, the rotating speed of the extruder is fixed at 200 r/min, the temperature is 180 ℃, the traction speed is 0.8m/min, the natural collapse distance of the unshaped sheet within 15cm from the die head is recorded, and the smaller the H is, the better the melt stiffness is.
(3) In the extrusion process, the rotating speed of the extruder is fixed at 200 r/min, the temperature is 180 ℃, the highest traction speed capable of stably extruding the sheet is recorded, and the higher the V is, the higher the extrusion efficiency is, and the more suitable the material is for extrusion molding.
Appearance: and observing the appearance condition of the workpiece, such as whether the glass fiber is exposed on the surface and whether the surface is smooth or not, by naked eyes. The surface of the product has no aggregation of spot-shaped glass fibers, and the silver-wire-shaped oriented floating fibers are difficult to observe as 'excellent'; slight glass fiber aggregation is observed on the surface of the workpiece, and slight silver filamentous orientation floating fiber is observed to be 'good'; the surface of the product has obvious spot-shaped glass fiber aggregation, and the obvious silver filamentous orientation floating fiber is easily observed to be 'poor'.
TABLE 1 EXAMPLES 1-10 formulations
TABLE 2 examples 11-21 formulations
TABLE 3 results of the Performance test of examples 1 to 10
TABLE 4 results of the Performance test of examples 11 to 21
TABLE 5 comparative examples 1-8 formulations
TABLE 6 Performance test results for comparative examples 1-8
By reasonable collocation of the components, a qualified material should meet the following requirements: tensile strength is more than or equal to 80MPa, and notch impact strength is more than or equal to 28KJ/m2T is more than or equal to 40s, H is less than 17mm, and V is more than or equal to 1 m/min;
further preferably, the material should fulfil the following requirements: tensile strength is more than or equal to 110MPa, and notch impact strength is more than or equal to 37KJ/m2T is more than or equal to 50s, H is less than 15mm, and V is more than or equal to 2 m/min.
Comparative example 1 in comparison with example 7, comparative example 1, in which no polyvinyl butyral was added, had poor extrudability and toughness, a cracking phenomenon occurred after a ball drop impact test, and the appearance of the material was rough.
Comparative examples 2 and 3 compared with example 7, the addition amount of the polyvinyl butyral in comparative example 2 exceeds the lower limit, which results in the decrease of "stiffness" and the deterioration of appearance of comparative example 2; the amount of polyvinyl butyral added in comparative example 3 exceeded the upper limit, resulting in a decrease in the "stiffness" of comparative example 3.
Comparative example 4 the polyethylene of comparative example 4 has an ethylene content of less than 18 wt% compared to example 15, resulting in deterioration of notched impact strength of comparative example 4 and occurrence of a ribbon breakage phenomenon during the production process.
Comparative example 5 compared with example 18, the number of parts of wollastonite in comparative example 5 exceeds the lower limit, resulting in deterioration of tensile strength, lowering of melt strength and lowering of extrusion efficiency in comparative example 5.
Comparative example 6 compared with example 18, the number of parts of wollastonite in comparative example 6 exceeds the upper limit, resulting in deterioration of tensile strength, lowering of melt strength, lowering of extrusion efficiency and deterioration of appearance roughness of comparative example 6.
Comparative example 7 compared with example 15, the number average molecular weight of the ultra-high molecular weight polyethylene of comparative example 7 was less than 150 ten thousand, and the melt strength of comparative example 7 was low, and the appearance was poor.
Comparative example 8 compared to example 15, comparative example 8, to which no ultra high molecular weight polyethylene was added, resulted in a decrease in melt strength and "stiffness" and poor appearance of comparative example 8, and also in the occurrence of strip breakage during production, which did not allow continuous production in the extrusion molding process.
Example 22
The long fiber reinforced polypropylene material of example 1 was tested as a bar with the following results: the tensile strength is 112MPa, and the notch impact strength is 35KJ/m2T is 50s, H is 14mm, V is 2.2m/min, and the surface is smooth and has no floating fiber. Therefore, the long fiber reinforced polypropylene material provided by the invention has excellent extrusion performance and good appearance and toughness, and can be well applied to extrusion molded products.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The long fiber reinforced polypropylene material is characterized by comprising the following components in parts by weight:
2. the long fiber-reinforced polypropylene material of claim 1, comprising the following components in parts by weight:
3. the long fiber reinforced polypropylene material of claim 1 or 2, wherein the wollastonite has an aspect ratio of (13-20): 1, the length-diameter ratio of the wollastonite is (15-18): 1.
4. the long fiber-reinforced polypropylene material of claim 1 or 2, wherein the polypropylene has an ethylene content of more than 18 wt%, preferably the polypropylene has an ethylene content of 21 to 24 wt%.
5. The long fiber-reinforced polypropylene material of claim 1 or 2, wherein the ultra-high molecular weight polyethylene has a number average molecular weight of more than 150 ten thousand.
6. The long fiber-reinforced polypropylene material of claim 1 or 2, further comprising 0.6 to 2 parts of an auxiliary agent.
7. The long fiber-reinforced polypropylene material of claim 6, wherein the additive is one or both of an antioxidant and a lubricant.
8. A method for preparing a long fiber-reinforced polypropylene material according to any one of claims 1 to 7, comprising the steps of:
s1: weighing the components according to the proportion, premixing the components except for the long glass fiber, putting the components into an extruder for melting plasticization and homogenization to form a melt, and finally conveying the melt to an impregnation die head;
s2: the traction equipment pulls the long glass fiber to pass through the impregnation die head, so that the continuous glass fiber is impregnated by the melt;
s3: and cooling, shaping and granulating the material strips obtained after the impregnation is finished to obtain the long fiber reinforced polypropylene material.
9. Use of the long fiber-reinforced polypropylene material according to any one of claims 1 to 7 in extrusion molded design products.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210288697.1A CN114621521B (en) | 2022-03-23 | 2022-03-23 | Long fiber reinforced polypropylene material and preparation method and application thereof |
| PCT/CN2023/082197 WO2023179487A1 (en) | 2022-03-23 | 2023-03-17 | Long fiber reinforced polypropylene material as well as preparation method therefor and use thereof |
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| CN202210288697.1A CN114621521B (en) | 2022-03-23 | 2022-03-23 | Long fiber reinforced polypropylene material and preparation method and application thereof |
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| CN114621521A true CN114621521A (en) | 2022-06-14 |
| CN114621521B CN114621521B (en) | 2023-10-17 |
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| WO (1) | WO2023179487A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023179487A1 (en) * | 2022-03-23 | 2023-09-28 | 江苏金发科技新材料有限公司 | Long fiber reinforced polypropylene material as well as preparation method therefor and use thereof |
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| JPH10298364A (en) * | 1997-04-24 | 1998-11-10 | Calp Corp | Reinforced polyolefin resin composition and formed article made of the composition |
| CN104592722A (en) * | 2015-02-03 | 2015-05-06 | 上海日之升新技术发展有限公司 | High-luster low-warpage glass fiber reinforced PBT/PP (Polybutylene Terephthalate/Polypropylene) alloy and preparation method thereof |
| CN106366443A (en) * | 2016-09-06 | 2017-02-01 | 株洲时代新材料科技股份有限公司 | Long glass fiber enhanced polypropylene material, and preparation method and application thereof |
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| US20050222303A1 (en) * | 2004-04-06 | 2005-10-06 | Cernohous Jeffrey J | Compositions and methods for producing highly filled materials |
| KR100666769B1 (en) * | 2005-10-17 | 2007-01-09 | 현대자동차주식회사 | Long fiber reinforced polypropylene composition and door shield module plate produced with the same |
| CN102532682B (en) * | 2010-12-16 | 2015-04-29 | 上海普利特复合材料股份有限公司 | Low-warpage high-glaze filling reinforcing polypropylene material and preparation method thereof |
| CN112760820B (en) * | 2020-12-23 | 2022-04-19 | 广东金发科技有限公司 | Melt-blown polypropylene material with long-acting soft hand feeling and preparation method and application thereof |
| CN114621521B (en) * | 2022-03-23 | 2023-10-17 | 江苏金发科技新材料有限公司 | Long fiber reinforced polypropylene material and preparation method and application thereof |
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2022
- 2022-03-23 CN CN202210288697.1A patent/CN114621521B/en active Active
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- 2023-03-17 WO PCT/CN2023/082197 patent/WO2023179487A1/en unknown
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| JPH10298364A (en) * | 1997-04-24 | 1998-11-10 | Calp Corp | Reinforced polyolefin resin composition and formed article made of the composition |
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| CN106366443A (en) * | 2016-09-06 | 2017-02-01 | 株洲时代新材料科技股份有限公司 | Long glass fiber enhanced polypropylene material, and preparation method and application thereof |
| CN110862618A (en) * | 2019-11-26 | 2020-03-06 | 上海纳岩新材料科技有限公司 | Ultra-low-warpage high-strength long glass fiber reinforced polypropylene composite material and preparation method thereof |
| CN112552595A (en) * | 2020-12-11 | 2021-03-26 | 上海金发科技发展有限公司 | High-strength high-toughness glass fiber reinforced polypropylene material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023179487A1 (en) * | 2022-03-23 | 2023-09-28 | 江苏金发科技新材料有限公司 | Long fiber reinforced polypropylene material as well as preparation method therefor and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114621521B (en) | 2023-10-17 |
| WO2023179487A9 (en) | 2023-11-16 |
| WO2023179487A1 (en) | 2023-09-28 |
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