CN112175296A - Recyclable basalt fiber reinforced polypropylene and preparation method thereof - Google Patents
Recyclable basalt fiber reinforced polypropylene and preparation method thereof Download PDFInfo
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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Abstract
The invention discloses recyclable basalt fiber reinforced polypropylene and a preparation method thereof, wherein the recyclable basalt fiber reinforced polypropylene comprises the following components: high-melting-index polypropylene, low-melting-index polypropylene, modified basalt fiber and processing aid. The recyclable basalt fiber reinforced polypropylene prepared by the invention is a polypropylene composition prepared by two different melt-index polypropylenes in a specific proportion under the modification effect of the modified basalt fiber, can be used in the field of building materials, has good mechanical properties, can be recycled, and has high performance retention rate after being recycled.
Description
Technical Field
The invention belongs to the field of building material high molecular polymers, and particularly relates to recyclable basalt fiber reinforced polypropylene and a preparation method thereof.
Background
In recent years, with the rapid development of urban construction in China, a large amount of high molecular polymers for building materials are rapidly developed. Polypropylene (PP) is a thermoplastic synthetic resin with excellent performance, and is colorless translucent thermoplastic light general-purpose plastic. The polypropylene has good chemical property, heat resistance, electrical insulation property, high-strength mechanical property, good high-wear-resistance processing property and the like, so that the polypropylene can be widely applied to the field of building materials.
With the rapid development of economy, the contradiction between human and environment is becoming more serious, and at the moment of rapid development of economy, the environmental problem becomes one of the biggest problems threatening the development of human survival. Due to the use of a large amount of building material high molecular polymers in the field of buildings, people are more eager for building materials capable of being developed sustainably to replace the existing materials.
However, the polypropylene has the disadvantages of poor mechanical properties after recycling, such as low strength and low weather resistance, resulting in poor recycling efficiency of the polypropylene composition.
Disclosure of Invention
The invention aims to provide recyclable basalt fiber reinforced polypropylene which is used in the field of building materials, has good mechanical properties, can be recycled, and still has excellent properties after being recycled.
Necessarily, the invention also provides a preparation method of the recyclable basalt fiber reinforced polypropylene.
A recyclable basalt fiber reinforced polypropylene comprises the following components:
high melt index polypropylene;
low melting means polypropylene;
modified basalt fibers;
a processing aid.
Preferably, the recyclable basalt fiber reinforced polypropylene comprises the following components in parts by weight:
more preferably, the recyclable basalt fiber reinforced polypropylene comprises the following components in parts by weight:
wherein the melt index of the high-melt-index polypropylene is 1000-2000g/10min, the test standard GB/T3682 is adopted, and the test condition is 230 ℃/2.16 kg.
Wherein the low-melting-index polypropylene has a melting index of 3-60g/10min, a test standard GB/T3682 and a test condition of 230 ℃/2.16 kg.
The modified basalt fiber is prepared by the following method:
mixing basalt fibers with a surface treatment agent in a ratio of (80-100): 0.7, and treating for 20-30 minutes at the temperature of 180-.
Wherein the content of magnesium element in the basalt fiber is 3-5%.
Preferably, the length-diameter ratio of the basalt fiber is 300-500, and the average diameter of the basalt fiber is 5-13 um.
Wherein the surface treatment agent is a mixture of dioctyl phthalate and a silane coupling agent.
Preferably, the weight ratio of dioctyl phthalate to silane coupling agent is 0.3: (0.3-0.5), more preferably, the weight ratio of the dioctyl phthalate and the silane coupling agent is 0.3: 0.4.
wherein the silane coupling agent is gamma-methacryloxypropyltrimethoxysilane.
The processing aid comprises an antioxidant and/or a pigment.
The antioxidant may be one or more antioxidants commonly used in the art, and may be selected from the group consisting of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1010), tris [2, 4-di-tert-butylphenyl ] phosphite (antioxidant 168), N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine (antioxidant 1098).
The preparation method of the recyclable basalt fiber reinforced polypropylene comprises the following steps:
1) mixing basalt fibers with a surface treatment agent in a ratio of (80-100): 0.7, and treating for 20-30 minutes at the temperature of 180-;
2) uniformly mixing the high-melt-index polypropylene, the low-melt-index polypropylene, the modified basalt fiber and the processing aid in a high mixing machine, adding the mixture into a double-screw extruder, carrying out melt extrusion, granulating and drying to obtain the recyclable basalt fiber reinforced polypropylene.
Preferably, the melt extrusion conditions are: the temperature of the first zone is 80-100 ℃, the temperature of the second zone is 210-; the length-diameter ratio of the twin-screw extruder is 40: 1.
Compared with the prior art, the recyclable basalt fiber reinforced polypropylene prepared by the invention has the advantages that under the modification effect of the modified basalt fiber, the viscosity of the whole system is lower due to the addition of the polypropylene with high melting index under the specific proportion of the polypropylene with two different melting indexes, so that the basalt fiber is subjected to weaker shearing in a screw, the strength of the polypropylene with low melting index is superior to that of the polypropylene with high melting index, and the resin strength of the material can be ensured due to the existence of part of the polypropylene with low melting index; the selected high-strength basalt fiber further improves the shearing resistance of the fiber through surface modification, the prepared polypropylene composition can be used in the field of building materials, the mechanical property is good, the polypropylene composition can be recycled, and the performance retention rate is high after the polypropylene composition is recycled.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the technical field better understand the scheme of the present invention.
Examples and comparative example raw material descriptions:
polypropylene A: the melt index is 1200g/10min, the manufacturer is Basel, the mark is MF650X, the test standard is GB/T3682, and the test condition is 230 ℃/2.16 kg;
polypropylene B: the melt index is 1800g/10min, the manufacturer is Basel, the mark is MF650Y, the test standard is GB/T3682, and the test condition is 230 ℃/2.16 kg;
polypropylene C: the melt index is 12g/10min, the manufacturer is Zhonghai shell brand, the brand is HP500N-Z, the test standard is GB/T3682, and the test condition is 230 ℃/2.16 kg;
polypropylene D: the melt index is 25g/10min, the manufacturer is named as petrochemical, the brand is N-Z30S, the test standard is GB/T3682, and the test condition is 230 ℃/2.16 kg;
basalt fiber E: 5 percent of magnesium element, 460 percent of length-diameter ratio, 13um of average diameter, and the manufacturer is Shijin and the brand is BCF-6-322;
basalt fiber F: 2 percent of magnesium element, 460 percent of length-diameter ratio, 13um of average diameter, and the manufacturer is Shijin and the brand is BCF-6-320;
basalt fiber G: 5 percent of magnesium element, the length-diameter ratio is 230, the average diameter is 13um, the manufacturer is Shijin, and the brand is BCF-3-322;
dioctyl phthalate: is sold on the market;
gamma-methacryloxypropyltrimethoxysilane: is sold on the market;
the processing aid is tris [2, 4-di-tert-butylphenyl ] phosphite, which is commercially available.
The rest raw materials are commercially available.
Example 1
The polypropylene composition was prepared as follows:
1) the mass ratio of the basalt fiber E to the surface treating agent (dioctyl phthalate and gamma-methacryloxypropyl trimethoxy silane is 3: 4) and (3) mixing the raw materials in a ratio of 90: 0.7, and treating for 30 minutes at the temperature of 200 ℃ and the stirring speed of 200 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃ and the temperature of the eighth zone is 220 ℃.
Example 2
The polypropylene composition was prepared as follows:
1) the mass ratio of the basalt fiber E to the surface treating agent (dioctyl phthalate and gamma-methacryloxypropyl trimethoxy silane is 1: 1) and (3) adding 80: 0.7, and treating for 20 minutes at the temperature of 180 ℃ and the stirring speed of 200 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
Example 3
The polypropylene composition was prepared as follows:
1) the mass ratio of the basalt fiber E to the surface treating agent (dioctyl phthalate and gamma-methacryloxypropyl trimethoxy silane is 3: 5) the method comprises the following steps of (1) dividing by 100: 0.7, and treating for 30 minutes at the temperature of 180 ℃ and the stirring speed of 180 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
Example 4
The polypropylene composition was prepared as follows:
1) the mass ratio of the basalt fiber E to the surface treating agent (dioctyl phthalate and gamma-methacryloxypropyl trimethoxy silane is 3: 4) and (3) mixing the raw materials in a ratio of 90: 0.7, and treating for 30 minutes at the temperature of 200 ℃ and the stirring speed of 200 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
Comparative example 1
The polypropylene composition was prepared as follows:
1) the mass ratio of the basalt fiber F to the surface treatment agent (dioctyl phthalate and gamma-methacryloxypropyl trimethoxy silane is 3: 4) and (3) mixing the raw materials in a ratio of 90: 0.7, and treating for 30 minutes at the temperature of 200 ℃ and the stirring speed of 200 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
Comparative example 2
The polypropylene composition was prepared as follows:
1) the mass ratio of the basalt fiber G to the surface treating agent (dioctyl phthalate and gamma-methacryloxypropyl trimethoxy silane is 3: 4) and (3) mixing the raw materials in a ratio of 90: 0.7, and treating for 30 minutes at the temperature of 200 ℃ and the stirring speed of 200 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
Comparative example 3
The polypropylene composition was prepared as follows:
1) the mass ratio of the basalt fiber E to the surface treating agent (dioctyl phthalate and gamma-methacryloxypropyl trimethoxy silane is 3: 4) and (3) mixing the raw materials in a ratio of 90: 0.7, and treating for 30 minutes at the temperature of 200 ℃ and the stirring speed of 200 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
Comparative example 4
The polypropylene composition was prepared as follows:
1) the mass ratio of the basalt fiber E to the surface treating agent (dioctyl phthalate and gamma-methacryloxypropyl trimethoxy silane is 3: 4) and (3) mixing the raw materials in a ratio of 90: 0.7, and treating for 30 minutes at the temperature of 200 ℃ and the stirring speed of 200 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
Comparative example 5
The polypropylene composition was prepared as follows:
1) the mass ratio of the basalt fiber E to the surface treating agent (dioctyl phthalate and gamma-methacryloxypropyl trimethoxy silane is 3: 4) and (3) mixing the raw materials in a ratio of 90: 0.7, and treating for 30 minutes at the temperature of 200 ℃ and the stirring speed of 200 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
Comparative example 6
The polypropylene composition was prepared as follows:
1) basalt fiber E was blended with gamma-methacryloxypropyltrimethoxysilane at a molar ratio of 90: 0.7, and treating for 30 minutes at the temperature of 200 ℃ and the stirring speed of 200 revolutions per minute to obtain modified basalt fibers;
2) polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the modified basalt fiber is fed into a double-screw extruder in a side feeding mode, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
Comparative example 7
The polypropylene composition was prepared as follows:
polypropylene and a processing aid are uniformly mixed in a high-speed mixer according to the weight parts shown in table 1, the basalt fiber is fed into a double-screw extruder on the side, and the polypropylene composition is obtained after melt extrusion, granulation and drying.
The conditions of melt extrusion were: the temperature of the first zone is 80 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 220 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 220 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, and the length-diameter ratio of the twin-screw extruder is 40: 1.
TABLE 1 EXAMPLES AND COMPARATIVE EXAMPLES raw materials recipe Table (unit: parts by weight)
The polypropylene compositions obtained in the examples and comparative examples were tested for the following properties and the test results are shown in Table 2:
tensile strength: ISO 527-1-2012, test rate 50 mm/min.
Bending strength: ISO 178-1-2010, test rate 2 mm/min.
Notched impact strength: standard ISO180-2001, cantilever beam.
Shear resistance: 50 g of polypropylene composition particles are placed in a crucible, then the crucible is placed in a muffle furnace at the temperature of 700 ℃ and is kept for 2h, after resin in the particles is burned out, the residual part is fiber, then the number average retention length of the fiber is tested, and the longer the retention length is, the better the shearing resistance is.
Performance testing after crushing cycle:
standing the polypropylene composition in an environment of 50-60 ℃ for 30 days, then placing the polypropylene composition outdoors for 30 days, crushing the polypropylene composition, performing melt extrusion by a double-screw extruder, granulating and drying, then testing the tensile strength, the notch impact strength, the bending strength and the shear resistance of the polypropylene composition according to the method, and comparing the tensile strength, the notch impact strength, the bending strength and the shear resistance with the tensile strength, the notch impact strength, the bending strength and the shear resistance before a crushing cycle to obtain the retention rates of the tensile strength, the notch impact strength, the bending strength and the fiber length.
TABLE 2 Polypropylene composition Performance test Table
The data show that the polypropylene composition prepared in the embodiments 1-4 of the invention selects the polypropylene with different melt fingers in a specific proportion, and the prepared polypropylene composition can be used in the field of building materials under the modification effect of the modified basalt fiber, so that the initial mechanical property is good, the polypropylene composition can be recycled, and the performance retention rate of the polypropylene composition after being recycled is high.
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. A recyclable basalt fiber reinforced polypropylene is characterized by comprising the following components:
high melt index polypropylene;
low melting means polypropylene;
modified basalt fibers;
a processing aid.
2. The recyclable basalt fiber-reinforced polypropylene according to claim 1, comprising the following components in parts by weight:
32-40 parts of high-melt-index polypropylene;
the low melting point means 14.5 to 22.5 weight parts of polypropylene;
40-50 parts of modified basalt fiber;
0-1 part of processing aid.
3. The recyclable basalt fiber-reinforced polypropylene of claim 2, wherein:
the melt index of the high-melt-index polypropylene is 1000-2000g/10min, the test standard GB/T3682.1-2018 is, and the test condition is 230 ℃/2.16 kg.
4. The recyclable basalt fiber-reinforced polypropylene of claim 2, wherein:
the low-melt-index polypropylene has a melt index of 3-60g/10min, a test standard GB/T3682.1-2018 and a test condition of 230 ℃/2.16 kg.
5. The recyclable basalt fiber-reinforced polypropylene according to claim 2, characterized in that the modified basalt fiber is produced by a method comprising:
mixing basalt fibers with a surface treatment agent in a ratio of (80-100): 0.7, and treating for 20-30 minutes at the temperature of 180-.
6. The recyclable basalt fiber-reinforced polypropylene of claim 5, wherein: the content of magnesium element in the basalt fiber is 3-5%.
7. The recyclable basalt fiber-reinforced polypropylene of claim 5, wherein: the length-diameter ratio of the basalt fiber is 300-500, and the average diameter of the basalt fiber is 5-13 um.
8. The recyclable basalt fiber-reinforced polypropylene of claim 5, wherein: the surface treating agent is a mixture of dioctyl phthalate and a silane coupling agent.
9. The recyclable basalt fiber-reinforced polypropylene of claim 8, wherein: the silane coupling agent is gamma-methacryloxypropyltrimethoxysilane.
10. A method for producing the basalt fiber-reinforced polypropylene recyclable according to any one of claims 1 to 9, characterized by comprising the steps of:
1) mixing basalt fibers with a surface treatment agent in a ratio of (80-100): 0.7, and treating for 20-30 minutes at the temperature of 180-;
2) uniformly mixing the high-melt-index polypropylene, the low-melt-index polypropylene, the modified basalt fiber and the processing aid in a high mixing machine, adding the mixture into a double-screw extruder, carrying out melt extrusion, granulating and drying to obtain the recyclable basalt fiber reinforced polypropylene.
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CN103289194A (en) * | 2013-05-22 | 2013-09-11 | 江苏金发科技新材料有限公司 | Basalt continuous fiber reinforced polypropylene material and preparation method thereof |
US20180118930A1 (en) * | 2016-10-28 | 2018-05-03 | Asahi Kasei Plastics North America, Inc. | Polyolefin resin composition |
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CN103289194A (en) * | 2013-05-22 | 2013-09-11 | 江苏金发科技新材料有限公司 | Basalt continuous fiber reinforced polypropylene material and preparation method thereof |
US20180118930A1 (en) * | 2016-10-28 | 2018-05-03 | Asahi Kasei Plastics North America, Inc. | Polyolefin resin composition |
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