CN112745576A - High-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene material and preparation method thereof - Google Patents

High-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene material and preparation method thereof Download PDF

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CN112745576A
CN112745576A CN202011611589.0A CN202011611589A CN112745576A CN 112745576 A CN112745576 A CN 112745576A CN 202011611589 A CN202011611589 A CN 202011611589A CN 112745576 A CN112745576 A CN 112745576A
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glass fiber
long glass
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王晶
张天荣
钱明娟
王凯
王明义
牛志海
卜祥星
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Shanghai Juwei New Material Co ltd
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Abstract

The invention discloses a long glass fiber reinforced polypropylene composite material with high heat resistance and high weather resistance and a preparation method thereof, belonging to the technical field of modification of high polymer materials. The high-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene composite material comprises the following components in parts by weight: 49-77.7 parts of PP, 0.5-5 parts of compatilizer, 0.2-2 parts of polar modifier, 20-50 parts of long glass fiber, 0.4-2.0 parts of antioxidant, 0.5-1.0 part of light stabilizer and 0.2-1.0 part of lubricant. By adding the polar modifier, the compatibility between PP and the long glass fiber is improved, and the strength and the modulus of the polypropylene are improved; adding high-efficiency compound antioxidant to reach 150 deg.C for over 1500hr for pulverization; by adding a compound light stabilizer without an antagonistic effect with the antioxidant, the weather resistance of the xenon lamp after aging for more than 2000hr can be achieved; meanwhile, the processing cost of the material is reduced, the quality of the material is improved, and the application range of the long glass fiber reinforced polypropylene composite material in the open air is widened.

Description

High-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene material and preparation method thereof
Technical Field
The invention belongs to the field of modification of high polymer materials, and particularly relates to a high-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene material and a preparation method thereof.
Background
The polypropylene long glass fiber reinforced material has excellent mechanical properties, especially excellent low-temperature notch impact performance, good dimensional stability, excellent fatigue resistance and low warping deformation, and can be used for outdoor plastic parts with high requirements on mechanical properties and dimensional stability. However, the polypropylene macromolecular chain has a large amount of unstable tertiary carbon atoms, so that the polypropylene macromolecular chain has the problems of surface cracking, chalking, stickiness, yellowing, discoloration and the like under the long-term sunlight exposure. In some high-demand parts such as automobile exterior parts, besides high mechanical property requirements, the long-acting heat resistance and long-acting weather resistance requirements are also very strict.
The patent (application publication No. CN201811652568.6) discloses 'an ultrahigh weather-resistant glass fiber mineral composite filling PP material and a preparation method thereof', the method adopts a light shielding agent, a UV absorbent, an antioxidant and the like to be used in glass fiber minerals, but the long-acting heat-resistant and weather-resistant effects achieved by the method are not clear. The patent (application publication No. 20120208374.5) discloses a weather-resistant and aging-resistant polypropylene material and a preparation method thereof, wherein the method adopts hindered amine and phosphite antioxidant, and benzotriazole light stabilizer and hindered amine light stabilizer. However, the requirements of long-acting heat resistance and long-acting weather resistance of exterior trimming parts in the modern automobile industry cannot be met. And with the increasing competition of the modified plastic industry, the cost reduction is in need.
Therefore, the technical problem to be solved by the technical personnel in the field is how to provide a preparation method of a long glass fiber reinforced polypropylene material with high heat resistance and high weather resistance.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a long glass fiber reinforced polypropylene material with high heat resistance and high weather resistance, wherein a long glass fiber impregnated die head device is introduced, a polar modifier is added, and then a suitable high-efficiency long-acting antioxidant and a light stabilizer which does not react with an ester antioxidant are selected to obtain a long glass fiber reinforced polypropylene composite material with high strength and high performance, and simultaneously, the long-acting heat resistance stability (the pulverization time at 150 ℃ is increased to 1500hr) and the long-acting weather resistance (the adopted wavelength is 340nm, and the irradiation intensity is 0.5W/m) of a PP material are ensured2And the weather resistance is evaluated by the change of 4-5 gray scale or color difference delta E before and after 102min drying and 18min water spraying and irradiation, and the weather resistance is improved to more than 2000 hr).
The long glass fiber is subjected to the working procedures of melting and dipping in a die head, cooling, traction and grain cutting, the obtained particle length is 6-25 mm, and the long glass fiber not only can keep a larger retention length, but also has better heat resistance (the high-temperature fatigue strength is twice of the common fatigue strength), better warping resistance and better low-temperature impact resistance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a high-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene composite material mainly comprises the following components in parts by weight:
Figure BDA0002874759110000021
preferably, the polypropylene resin is isotactic polypropylene, atactic polypropylene, syndiotactic polypropylene, ethylene-propylene copolymer or cross-linked modified polypropylene. More preferably, the polypropylene resin is isotactic polypropylene.
Preferably, the compatibilizer comprises at least one of PP grafted maleic anhydride, POE grafted glycidyl methacrylate, styrene-acrylonitrile-maleic anhydride copolymer and ethylene-butadiene-styrene triblock copolymer grafted maleic anhydride.
More preferably, the compatilizer is PP grafted maleic anhydride and is prepared by adopting a solution method for polymerization, wherein the maleic anhydride content is 5% and is more than 1-2% of the common maleic anhydride content.
Preferably, the polar modifier comprises at least one of ethylene-methyl acrylate copolymer, ethylene-butyl acrylate copolymer, ethylene-vinyl acetate copolymer, ethylene-ethyl acrylate copolymer, ethylene-maleic anhydride copolymer and ethylene-glycidyl acrylate copolymer.
Further preferably, the polar compatilizer is a blend of ethylene-maleic anhydride copolymer and ethylene-vinyl acetate copolymer, wherein the content of the copolymer of maleic anhydride and vinyl acetate is more than 10%.
The long glass fiber is alkali-free glass fiber with the surface treated by a coupling agent and a film forming agent.
Preferably, the antioxidant comprises at least pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], N' -1, 6-hexylene-bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionamide ], N-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 1,3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzyl) -1,3, 5-triazine-2, 4,6- (1H,3H,5H) trione, triethylene glycol bis [3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], 2,2 '-methylenebis (4-methyl-6-tert-butylphenol), tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, dioctadecylpentaerythritol diphosphite, tetrakis (2, 4-di-tert-butylphenyl-4, 4' -biphenyl) bisphosphonate, pentaerythritol tetrakis (3-laurylthiopropionate).
Further preferably, the antioxidant is at least one of 1,3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzyl) -1,3, 5-triazine-2, 4,6- (1H,3H,5H) trione, bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite and pentaerythritol tetrakis (3-laurylthiopropionate).
Preferably, the light stabilizer includes at least carbon black, zinc oxide, 2-hydroxy-4-n-octoxybenzophenone, 2- (2' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole, 2- (2' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole, 2- (2' -hydroxy-5 ' -tert-octylphenyl) benzotriazole, 2' -methylenebis (6- (2H-benzotriazol-2-yl) -4- (1,1,3, 3-tetramethylbutyl) phenol), 2- (benzotriazol-2-yl) -4- (5,5 '-dimethylhexyl) -6- (2' -hydroxy-3 '-tert-butyl-5' -methylbenzyl) phenol, 1,5,8, 12-tetrakis [4, 6-bis (N-butyl-N-1, 2,2,6, 6-pentamethyl-4-piperidinylamino) -1,3, 5-triazin-2-yl ] -1,5,8, 12-tetraazadodecane 119FL, bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate, polysuccinic acid (4-hydroxy-2, 2,6, 6-tetramethyl-1-piperidineethanol), Chimassorb 944, 2,2,6, 6-tetramethyl-4-piperidineacrylate, Chimasorb, One of N, N '-diformyl-N, N' -bis (2,2,6, 6-tetramethyl-4-piperidine) -hexamethylenediamine, 2,6, 6-tetramethylpiperidinol ester, NOR 116, and N-hexadecyl 3, 5-di-tert-butyl-4-hydroxybenzoate.
Further preferably, the light stabilizer is a compound of two or three of 2- (benzotriazol-2-yl) -4- (5,5 '-dimethylhexyl) -6- (2' -hydroxy-3 '-tert-butyl-5' -methylbenzyl) phenol JAST-500, N-hexadecyl 3, 5-di-tert-butyl-4-hydroxybenzoate 2908, and 1,5,8, 12-tetrakis [4, 6-bis (N-butyl-N-1, 2,2,6, 6-pentamethyl-4-piperidinylamino) -1,3, 5-triazin-2-yl ] -1,5,8, 12-tetraazadodecane 119 FL.
Preferably, the lubricant at least comprises one of polyethylene wax, N '-ethylene bisstearamide, organic silicone oil, oleamide, ethylene bisoleamide, N' -ethylene bisstearamide-grafted maleic anhydride, silicone powder and fluorine-containing lubricant.
Further preferably, the lubricant is at least one of silicone oil and N, N' -ethylene bisstearamide-grafted maleic anhydride.
The application also claims a preparation method of the high-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene composite material, which comprises the following specific steps:
s1, penetrating the long glass fiber into a special impregnation die head;
s2, putting the raw materials except the long glass fibers into a high-speed mixer, stirring and mixing at the rotating speed of 80-100rpm for 3-4min, and uniformly mixing;
and S3, melting the obtained mixture through a double-screw extruder, and then passing through a special glass fiber die head to obtain the polypropylene composite material.
Preferably, the temperature of each section of the double-screw extruder is controlled to be 190-290 ℃, and the screw rotating speed is set to be 200-350rpm for granulation.
Further preferably, the temperature of each section of the main machine cylinder is controlled in a segmented mode, the temperature from the feed inlet to the outlet of the machine head is 190 ℃, 200 ℃, 210 ℃, 270 ℃, 280 ℃, 290 ℃ and 280 ℃ in sequence, and the rotating speed of the double-screw extruder is 300 revolutions per minute.
The high-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene composite material is prepared by injection molding modified polypropylene particles into ISO sample strips, controlling the temperature of each section of the injection molding machine to be 150-250 ℃, and testing the mechanical properties such as surface energy, tensile strength, bending modulus and the like.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
according to the invention, the special impregnation die head for the long fiber is introduced, so that the cut glass fiber keeps a longer retention length, the polar modifier is added, and then the proper high-efficiency compound antioxidant and the compound light stabilizer which does not react with the ester antioxidant are selected, so that the glass fiber reinforced polypropylene composite material with high mechanical property, high heat resistance and strong weather resistance is obtained. The technical scheme disclosed and protected by the invention can achieve the following technical indexes:
1) and (3) weather resistance test: the gray scale of 2000hr is 4-5,
2) and (3) heat resistance test: the powder is not pulverized at the temperature of 150 ℃/1500hr,
3) the tensile strength is more than 110MPa,
4) the bending strength is more than 140MPa,
5) the flexural modulus is more than 6000MPa,
6) notched impact strength>20kJ/m2。
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.
The raw materials used in the examples: PP is S2040 (Siccaceae, homopolymerization type), PP grafted maleic anhydride is H-1000P (Japan Toyobo, copolymerization type, maleic anhydride content is 5%), ethylene-maleic anhydride copolymer is 1125AC (U.S. DuPont, copolymerization type, maleic anhydride content is 25%), glass fiber is 988 (megastone, alkali-free glass fiber, continuous type), antioxidant is a compound of 1790 (Korean pine origin), 626 (Shanghai Kai chemical industry) and 412S (Korea), light stabilizer is a compound of 2908 (American cyante), JAST-500 (Japanese North chemical industry) and 119FL (U.S. Basf), and lubricant is TAF (commercially available).
Example 1
The embodiment 1 of the invention discloses a preparation method of a long glass fiber reinforced polypropylene composite material with high heat resistance and high weather resistance, which adopts the following technical scheme:
the specific weight fraction ratio of each component is S2040: 77.4 parts; H-1000P: 0.5 part; 1125 AC: 0.2 part, 1790: 0.1 part, 626: 0.2 part, 412S: 0.3%, 2908:0.2 parts, JAST-500: 0.3 part, 119 FL: 0.2 part, 0.4 part of carbon black, ZnO: 0.2 part of long glass fiber: 20 parts of (1);
firstly, adding PP, H-1000P, 1125AC, an antioxidant, a light stabilizer and a lubricant into a high-speed mixer according to the proportion, mixing for 3min, then extruding and granulating the uniformly mixed materials through a double-screw extruder, allowing long glass fibers to penetrate into an impregnation die head to obtain modified particles, and setting the temperature of each section of the extruder temperature as follows: 190 ℃, 200 ℃, 210 ℃, 270 ℃, 280 ℃, 290 ℃, 280 ℃, and the screw speed is set to 300 rpm.
The injection molding temperature is 250 ℃, 240 ℃ and 230 ℃, and ISO sample strips are prepared for testing.
Example 2
The embodiment 2 of the invention discloses a preparation method of a long glass fiber reinforced polypropylene composite material with high heat resistance and high weather resistance, which adopts the following technical scheme:
the specific weight fraction ratio of each component is S2040: 66.3 parts; H-1000P: 1 part; 1125 AC: 0.5 part, 1790: 0.3 part, 626: 0.1 part, 412S: 0.6 part, 2908:0.3 part, JAST-500: 0.2 part, 119 FL: 0.2 part, 0.5 part of carbon black, and glass fiber: 30 parts of (1);
firstly, adding PP, H-1000P, 1125AC, an antioxidant, a light stabilizer and a lubricant into a high-speed mixer according to the proportion, mixing for 3min, then extruding and granulating the uniformly mixed materials through a double-screw extruder, allowing long glass fibers to penetrate into an impregnation die head to obtain modified particles, and setting the temperature of each section of the extruder to be: 190 ℃, 200 ℃, 210 ℃, 270 ℃, 280 ℃, 290 ℃, 280 ℃, and the screw speed is set to 350 rpm.
The injection molding temperature is 250 ℃, 240 ℃ and 230 ℃, and ISO sample strips are prepared for testing.
Example 3
The embodiment 3 of the invention discloses a preparation method of a long glass fiber reinforced polypropylene composite material with high heat resistance and high weather resistance, which adopts the following technical scheme:
the specific weight fraction ratio of each component is S2040: 52.4 parts; H-1000P: 3 parts of a mixture; 1125 AC: 1.0 part, 1790: 0.7 part, 626: 0.2 part, 412S: 0.9 parts, 2908:0.2 parts, JAST-500: 0.5 part, 119 FL: 0.3 part, 0.8 part of carbon black, and glass fiber: 40 parts of a mixture;
firstly, adding PP, H-1000P, 1125AC, an antioxidant, a light stabilizer and a lubricant into a high-speed mixer according to the proportion, mixing for 3min, then extruding and granulating the uniformly mixed materials through a double-screw extruder, allowing long glass fibers to penetrate into an impregnation die head to obtain modified particles, and setting the temperature of each section of the extruder to be: 190 ℃, 200 ℃, 210 ℃, 270 ℃, 280 ℃, 290 ℃, 280 ℃, and the screw speed is set to 350 rpm.
The injection molding temperature is 250 ℃, 240 ℃ and 230 ℃, and ISO sample strips are prepared for testing.
To further verify the excellent effects achieved by the technical solutions disclosed in the present application, the inventors have also performed the following test experiments:
the tensile strength is tested according to ISO527, the bending strength and the bending modulus are tested according to ISO178, the notched impact strength is tested according to ISO179, and the thermal aging at 150 ℃ is tested according to 5.14 in the popular VW44045 standard; illumination was tested according to SAEJ 2527.
TABLE 1
Example 1 Example 2 Example 3 Comparative example
Tensile Strength (MPa) 110 130 150 105
Flexural Strength (MPa) 140 160 190 130
Flexural modulus (MPa) 6000 7000 12000 5000
Notched impact strength (kJ/m2) 22 28 32 15
Powdering time at 150 ℃ 1620 1730 1789 750
Gray scale value after 2000hr of illumination 4～5 4～5 4～5 2～4
In summary, the long glass fiber reinforced polypropylene composite material with high heat resistance and high weather resistance provided by the invention is prepared by introducing a long fiber dipping device, adding a polar modifier, and selecting a proper high-efficiency compound antioxidant and a compound light stabilizer which does not react with an ester antioxidant, so as to finally obtain the glass fiber reinforced polypropylene composite material with high mechanical property, high heat resistance and strong weather resistance.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. The high-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene composite material is characterized by mainly comprising the following components in parts by weight:
Figure FDA0002874759100000011
2. the long glass fiber reinforced polypropylene composite material with high heat resistance and high weather resistance as claimed in claim 1, wherein the polypropylene resin is isotactic polypropylene, atactic polypropylene, syndiotactic polypropylene, ethylene-propylene copolymer or cross-linked modified polypropylene.
3. The high heat and weather resistant long glass fiber reinforced polypropylene composite material as claimed in claim 1, wherein the compatibilizer comprises at least one of PP grafted maleic anhydride, POE grafted glycidyl methacrylate, styrene-acrylonitrile-maleic anhydride copolymer, and ethylene-butadiene-styrene triblock copolymer grafted maleic anhydride.
4. The high heat and weather resistant long glass fiber reinforced polypropylene composite material as claimed in claim 1, wherein the polar modifier comprises at least one of ethylene-methyl acrylate copolymer, ethylene-butyl acrylate copolymer, ethylene-vinyl acetate copolymer, ethylene-ethyl acrylate copolymer, ethylene-maleic anhydride copolymer, and ethylene-glycidyl acrylate copolymer.
5. The high heat and weather resistant long glass fiber reinforced polypropylene composite material as claimed in claim 1, wherein the antioxidant comprises at least pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], N' -1, 6-hexylene-bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionamide ], N-octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 1,3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzyl) -1,3, 5-triazine-2, 4,6- (1H,3H,5H) trione, triethylene glycol bis [3- (3-tert-butyl-4-hydroxy-5-methyl ethyl ketone ] Phenyl) propionate ], 2 '-methylenebis (4-methyl-6-tert-butylphenol), tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, dioctadecylpentaerythritol diphosphite, tetrakis (2, 4-di-tert-butylphenyl-4, 4' -biphenyl) bisphosphonate, pentaerythritol tetrakis (3-laurylthiopropionate).
6. The highly heat-resistant, highly weather-resistant long glass fiber reinforced polypropylene composite material according to claim 1, wherein the light stabilizer comprises at least carbon black, zinc oxide, 2-hydroxy-4-n-octoxybenzophenone, 2- (2' -hydroxy-3 ' -tert-butyl-5 ' -methylphenyl) -5-chlorobenzotriazole, 2- (2' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole, 2- (2' -hydroxy-5 ' -tert-octylphenyl) benzotriazole, 2' -methylenebis (6- (2H-benzotriazol-2-yl) -4- (1,1,3, 3-tetramethylbutyl) phenol), and mixtures thereof, 2- (benzotriazol-2-yl) -4- (5,5 '-dimethylhexyl) -6- (2' -hydroxy-3 '-tert-butyl-5' -methylbenzyl) phenol, 1,5,8, 12-tetrakis [4, 6-bis (N-butyl-N-1, 2,2,6, 6-pentamethyl-4-piperidinylamino) -1,3, 5-triazin-2-yl ] -1,5,8, 12-tetraazadodecane 119FL, bis (2,2,6, 6-tetramethyl-4-piperidinyl) sebacate, polysuccinic acid (4-hydroxy-2, 2,6, 6-tetramethyl-1-piperidineethanol) ester, and mixtures thereof, One of Chimassorb 944, 2,6, 6-tetramethyl-4-piperidine stearate, N '-diformyl-N, N' -bis (2,2,6, 6-tetramethyl-4-piperidine) -hexamethylenediamine, 2,6, 6-tetramethylpiperidinol ester, NOR 116, and N-hexadecyl 3, 5-di-tert-butyl-4-hydroxybenzoate.
7. The high heat and weather resistant long glass fiber reinforced polypropylene composite material as claimed in claim 1, wherein the lubricant comprises at least one of polyethylene wax, N '-ethylene bis stearamide, silicone oil, oleamide, ethylene bis oleamide, N' -ethylene bis stearamide-grafted maleic anhydride, silicone powder and fluorine-containing lubricant.
8. The preparation method of the high heat-resistant and high weather-resistant long glass fiber reinforced polypropylene composite material as claimed in claim 1, wherein the method comprises the following steps:
s1, weighing the raw materials according to the weight ratio of claim 1 for later use;
s2, adding the raw materials weighed in the step S1 except the long glass fibers into a high-speed mixer for mixing, continuously and uniformly adding the mixed materials into a main machine cylinder of a double-screw extruder by using a double-screw feeder, uniformly coating the molten materials extruded from the extruder on the surface of the long glass fibers by using the long glass fibers through a melting impregnation die head, cooling the extruded material strips through a water tank, then pelletizing, and pelletizing to obtain particles with the length of 6-25 mm, thereby obtaining the high-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene composite material.
9. The method for preparing the high heat-resistant and high weather-resistant long glass fiber reinforced polypropylene composite material as claimed in claim 8, wherein the temperature of each section of the twin-screw extruder is controlled to be 150 ℃ to 250 ℃, and the rotating speed of the twin-screw extruder is 200 rpm to 350 rpm.
10. The method for preparing the high heat-resistant and high weather-resistant long glass fiber reinforced polypropylene composite material as claimed in claim 8 or 9, wherein the temperature of each section of the main barrel is controlled in a segmented manner, the temperature is 190 ℃, 200 ℃, 210 ℃, 270 ℃, 280 ℃, 290 ℃ and 280 ℃ from the feed inlet to the outlet of the machine head in sequence, and the rotating speed of the twin-screw extruder is 300 revolutions per minute.
CN202011611589.0A 2020-12-30 2020-12-30 High-heat-resistance and high-weather-resistance long glass fiber reinforced polypropylene material and preparation method thereof Pending CN112745576A (en)

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