CN115895248A - Nylon polyphenyl ether composite material and preparation method and application thereof - Google Patents
Nylon polyphenyl ether composite material and preparation method and application thereof Download PDFInfo
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- CN115895248A CN115895248A CN202211506943.2A CN202211506943A CN115895248A CN 115895248 A CN115895248 A CN 115895248A CN 202211506943 A CN202211506943 A CN 202211506943A CN 115895248 A CN115895248 A CN 115895248A
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- 229920001778 nylon Polymers 0.000 title claims abstract description 86
- 239000004677 Nylon Substances 0.000 title claims abstract description 82
- 239000002131 composite material Substances 0.000 title claims abstract description 71
- 229920013636 polyphenyl ether polymer Polymers 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 55
- 229920005989 resin Polymers 0.000 claims abstract description 33
- 239000011347 resin Substances 0.000 claims abstract description 33
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 26
- 229920006380 polyphenylene oxide Polymers 0.000 claims abstract description 26
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 24
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 16
- 229920001955 polyphenylene ether Polymers 0.000 claims description 38
- 239000002667 nucleating agent Substances 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 21
- 238000002844 melting Methods 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 16
- 239000007822 coupling agent Substances 0.000 claims description 15
- 239000003963 antioxidant agent Substances 0.000 claims description 14
- 230000003078 antioxidant effect Effects 0.000 claims description 14
- 239000000314 lubricant Substances 0.000 claims description 14
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical group O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 14
- 229920006111 poly(hexamethylene terephthalamide) Polymers 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 12
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- 229920000578 graft copolymer Polymers 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 6
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 6
- DJZKNOVUNYPPEE-UHFFFAOYSA-N tetradecane-1,4,11,14-tetracarboxamide Chemical compound NC(=O)CCCC(C(N)=O)CCCCCCC(C(N)=O)CCCC(N)=O DJZKNOVUNYPPEE-UHFFFAOYSA-N 0.000 claims description 6
- GVNWZKBFMFUVNX-UHFFFAOYSA-N Adipamide Chemical compound NC(=O)CCCCC(N)=O GVNWZKBFMFUVNX-UHFFFAOYSA-N 0.000 claims description 4
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical group [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 4
- WBWXVCMXGYSMQA-UHFFFAOYSA-N 3,9-bis[2,4-bis(2-phenylpropan-2-yl)phenoxy]-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound C=1C=C(OP2OCC3(CO2)COP(OC=2C(=CC(=CC=2)C(C)(C)C=2C=CC=CC=2)C(C)(C)C=2C=CC=CC=2)OC3)C(C(C)(C)C=2C=CC=CC=2)=CC=1C(C)(C)C1=CC=CC=C1 WBWXVCMXGYSMQA-UHFFFAOYSA-N 0.000 claims description 3
- 229910021595 Copper(I) iodide Inorganic materials 0.000 claims description 3
- 229920000571 Nylon 11 Polymers 0.000 claims description 3
- 229920000299 Nylon 12 Polymers 0.000 claims description 3
- 229920002292 Nylon 6 Polymers 0.000 claims description 3
- 229920000305 Nylon 6,10 Polymers 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 150000008430 aromatic amides Chemical class 0.000 claims description 3
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical class C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical compound I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 claims description 3
- 229920001971 elastomer Polymers 0.000 claims description 3
- 239000000806 elastomer Substances 0.000 claims description 3
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 claims description 3
- 125000000623 heterocyclic group Chemical group 0.000 claims description 3
- SYECJBOWSGTPLU-UHFFFAOYSA-N hexane-1,1-diamine Chemical compound CCCCCC(N)N SYECJBOWSGTPLU-UHFFFAOYSA-N 0.000 claims description 3
- 229920001910 maleic anhydride grafted polyolefin Polymers 0.000 claims description 3
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 3
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 3
- 125000003107 substituted aryl group Chemical group 0.000 claims description 3
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims 2
- 235000019260 propionic acid Nutrition 0.000 claims 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003960 organic solvent Substances 0.000 abstract description 5
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- 230000000052 comparative effect Effects 0.000 description 17
- 238000012360 testing method Methods 0.000 description 12
- 229920000642 polymer Polymers 0.000 description 9
- 239000004952 Polyamide Substances 0.000 description 7
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- 238000005299 abrasion Methods 0.000 description 6
- 239000000956 alloy Substances 0.000 description 5
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- MHSKRLJMQQNJNC-UHFFFAOYSA-N terephthalamide Chemical compound NC(=O)C1=CC=C(C(N)=O)C=C1 MHSKRLJMQQNJNC-UHFFFAOYSA-N 0.000 description 3
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 description 2
- FQLAJSQGBDYBAL-UHFFFAOYSA-N 3-(azepane-1-carbonyl)benzamide Chemical compound NC(=O)C1=CC=CC(C(=O)N2CCCCCC2)=C1 FQLAJSQGBDYBAL-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
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- QZUPTXGVPYNUIT-UHFFFAOYSA-N isophthalamide Chemical compound NC(=O)C1=CC=CC(C(N)=O)=C1 QZUPTXGVPYNUIT-UHFFFAOYSA-N 0.000 description 2
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- NIXONLGLPJQPCW-UHFFFAOYSA-K gold trifluoride Chemical compound F[Au](F)F NIXONLGLPJQPCW-UHFFFAOYSA-K 0.000 description 1
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Abstract
The invention relates to a nylon polyphenylene oxide composite material and a preparation method and application thereof. The composite material comprises the following components in percentage by mass: 20 to 60 percent of nylon resin; 10 to 50 percent of polyphenyl ether resin; 3% -10% of a compatilizer; 5 to 50 percent of potassium titanate whisker; and 5% -20% of polytetrafluoroethylene micro powder; the diameter of the potassium titanate whisker is 0.1-2 mu m, and the length is 1-100 mu m; the particle size of the polytetrafluoroethylene micro powder is less than 200 mu m, and the D50 particle size is less than 40 mu m. The nylon polyphenyl ether composite material is wear-resistant, high-strength, high-temperature-resistant, low in water absorption, stable in size and resistant to organic solvents, and can meet the requirements of industries such as automobiles, electronic appliances and the like on high-performance high-quality appearance composite materials.
Description
Technical Field
The invention relates to the field of polymer composite materials, in particular to a nylon polyphenylene oxide composite material and a preparation method and application thereof.
Background
Polyamide (PA), commonly known as nylon, is a crystalline polymer containing an amide bond (-NHCO-) in the main molecular chain, and has high mechanical strength, good fluidity, good toughness, self-lubrication, good friction resistance, excellent heat resistance, electrical properties, and weather resistance, but has the disadvantages of easy water absorption, poor dimensional stability (large shrinkage), and the like, and thus the application of Polyamide (PA) is limited.
Polyphenylene Oxide (PPO) resin is an amorphous thermoplastic polymer, and has the defects of high mechanical strength, high temperature resistance, low specific gravity, low water absorption, excellent hydrolysis resistance, excellent dimensional stability and excellent electrical property, but poor flowability, poor organic solvent resistance and the like, so that the application of the PPO resin is limited.
The polymer alloy is a material with uniform appearance and containing a multi-component polymer system with two or more different structures, can improve the physical and mechanical properties and the processing property of a high polymer material, reduce the cost and enlarge the application range, and is one of important ways for realizing polymer modification and producing a new multi-property material. Although many polymer alloys have been reported, there is currently less research on polymer alloys compounded with nylon and polyphenylene ether.
Disclosure of Invention
Therefore, in order to solve the above problems, it is necessary to provide a nylon polyphenylene oxide composite material which is wear-resistant, high-strength, high-temperature resistant, low in water absorption, stable in size, and resistant to organic solvents, and can meet the requirements of industries such as automobiles, electronic appliances and the like on high-performance and high-quality appearance composite materials.
The technical scheme is as follows:
a nylon polyphenylene oxide composite material comprises the following components in percentage by mass:
the diameter of the potassium titanate whisker is 0.1-2 μm, and the length is 1-100 μm;
the particle size of the polytetrafluoroethylene micro powder is less than 200 mu m, and the particle size of D50 is less than 40 mu m.
In one embodiment, the potassium titanate whisker has a diameter of 0.1 to 1 μm and a length of 10 to 20 μm.
In one embodiment, the chemical composition of the potassium titanate whisker is K 2 O·2TiO 2 、K 2 O·4TiO 2 、K 2 O·6TiO 2 And K 2 O·8TiO 2 One or more of them.
In one embodiment, the polyphenylene ether resin has a Ubbelohde intrinsic viscosity of 0.2dl/g to 0.8dl/g in chloroform at 25 ℃.
In one embodiment, the compatibilizer is a maleic anhydride grafted polymer with a grafting ratio of 0.5% to 5.0%.
In one embodiment, the maleic anhydride grafted polymer is selected from one or more of a mixture of maleic anhydride grafted polyolefin elastomer, maleic anhydride grafted hydrogenated styrene-butadiene block copolymer, and maleic anhydride grafted polyphenylene ether.
In one embodiment, the nylon resin is selected from semi-crystalline nylons having a melting point of aliphatic and/or semi-aromatic.
In one embodiment, the nylon resin is selected from the group consisting of polycaprolactam, polytetramethylene adipamide, polypentamethyleneadipamide, polyhexamethylene adipamide, polyhexamethylene sebacamide, polyhexamethylene dodecacarbodiimide, polyundecanolactam, polydodecanolactam, polydodecanodidodecacarbodiimide, copolynylhexamethylene terephthalamide/isophthalamide, copolynylnylon of polyhexamethylene terephthalamide/hexamethylene adipamide, copolynylnylon of polyhexamethylene terephthalamide/hexamethylene isophthalamide/hexamethylene adipamide, copolynylnylon of polyhexamethylene terephthalamide/caprolactam, copolynylnylon of polyhexamethylene terephthalamide/2-methylpentamethylene terephthalamide, polyparanonanediphthalamide, and mixtures of one or more of them.
In one embodiment, the nylon polyphenylene oxide composite material further comprises one or more of an antioxidant, a lubricant, a nucleating agent and a coupling agent.
In one embodiment, the nylon polyphenylene oxide composite material further comprises 0.2-0.5% of antioxidant in percentage by mass; 0.1 to 0.5 percent of lubricant; 0.1 to 1 percent of nucleating agent; and 0.1 to 1 percent of coupling agent.
In one embodiment, the antioxidant is selected from N, N' -1, 6-hexylene-bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionamide]、
S9228, tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid]Pentaerythritol ester, N' -bis- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-dicumylphenyl) pentaerythritol diphosphite, potassium iodide and cuprous iodide.
In one embodiment, the lubricant is one or more of calcium stearate, N' -ethylene bis stearamide, ethylene acrylic acid copolymer, OP wax and E wax.
In one embodiment, the nucleating agent is selected from one or a mixture of several of long carbon chain carboxylate nucleating agents, substituted aryl heterocyclic phosphate nucleating agents, aryl carboxylate nucleating agents and aromatic amide nucleating agents.
In one embodiment, the coupling agent is an aminosilane-based coupling agent.
The invention also provides a preparation method of the nylon polyphenylene oxide composite material, which comprises the following steps:
and mixing, melting and extruding the nylon resin, the polyphenyl ether resin, the compatilizer, the potassium titanate whisker and the polytetrafluoroethylene micro powder.
The invention also provides application of the nylon polyphenylene oxide composite material. The technical scheme is as follows:
an electronic appliance comprising the nylon polyphenylene ether composite material as described above.
An automobile comprising a nylon polyphenylene ether composite as described above.
The invention has the following beneficial effects:
the nylon polyphenyl ether composite material disclosed by the invention is prepared by compounding nylon and polyphenyl ether, and adopting the compatilizer, the potassium titanate whisker and the polytetrafluoroethylene micropowder in a matching manner, so that the performance defects of each single resin can be obviously improved, and the alloy material with excellent and balanced performances such as wear resistance, mechanical property, processability, temperature resistance, chemical resistance, hydrolysis resistance, dimensional stability and the like is obtained. Furthermore, the potassium titanate whisker and the polytetrafluoroethylene micro powder are matched to reinforce the filling material, so that the appearance of the material which is better than the appearance of the conventional glass fiber, carbon fiber and mineral powder filled and reinforced material can be obtained, the glossiness of the material is higher, the wear resistance is better, the dimensional stability is better, the application fields of nylon and polyphenyl ether materials are greatly widened, and the material can be applied to the fields of electronic appliances and automobiles, and particularly can be applied to high-temperature-resistant and wear-resistant parts with high precision requirements such as vehicle-mounted cameras, sliders and gears.
Drawings
FIG. 1 is a graph showing the effect of the nylon polyphenylene ether composite material prepared in comparative example 3 after a friction test;
FIG. 2 is a graph showing the effect of the nylon polyphenylene ether composite material obtained in example 2 after a friction test.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the present invention, the technical features described in the open type include a closed technical solution including the listed features, and also include an open technical solution including the listed features.
In the present invention, the numerical intervals are regarded as continuous, and include the minimum and maximum values of the range and each value between such minimum and maximum values, unless otherwise specified. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.
The temperature parameter in the present invention is not particularly limited, and may be a constant temperature treatment or a treatment within a certain temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control.
In the present invention, referring to the units of the data range, if only the right end point is followed by a unit, the units indicating the left end point and the right end point are the same. For example, 150 to 160 ℃ means that the units of the left end point "150 and the right end point" 160 "are both in degrees centigrade.
In the present invention, in the description of the invention, "several" means at least two, for example, two, three, etc., unless explicitly defined otherwise. In the description of the present application, "a number" means at least one, such as one, two, etc., unless specifically limited otherwise.
All embodiments and alternative embodiments of the invention may be combined with each other to form new solutions, if not specifically stated.
All steps of the present invention may be performed sequentially or randomly, preferably sequentially, if not specifically stated. For example, the method comprises steps (a) and (b), meaning that the method may comprise steps (a) and (b) performed sequentially, and may also comprise steps (b) and (a) performed sequentially. For example, said reference to said process may also include step (c), meaning that step (c) may be added to said process in any order, for example, said process may include steps (a), (b) and (c), may also include steps (a), (c) and (b), may also include steps (c), (a) and (b), etc.
It should be noted that in the description of the present invention, for the terms of orientation, there are terms such as "central", "lateral", "longitudinal", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise" and the like indicating the orientation and positional relationship based on the orientation or positional relationship shown in the drawings, which are only for the convenience of describing the present invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and should not be construed as limiting the specific scope of the present invention.
Where the terms "comprising," "having," and "including" are used herein, it is intended to cover a non-exclusive inclusion, as another element may be added, unless an explicit limitation is used, such as "only," "consisting of 8230; \8230; composition," etc.
Unless mentioned to the contrary, terms in the singular may include the plural and are not to be construed as being one in number.
In the present invention, the graft ratio refers to the mass ratio of the polar monomer grafted to the polymer to the mass of the polymer after grafting.
Potassium Titanate Whiskers (PTW) were originally needle-shaped artificial fibers developed by DuPont, USA, and the main chemical component was K 2 O·nTiO 2 (n is an integer greater than 0), has a diameter of several micrometers or less, a length of several tens of micrometers or less, and a certain major axisRatio (general L/D)>20). It is different from general powder filler, and its fibrous microstructure can make it possess obvious reinforcing effect when it is used as filler and filled in high-molecular material, and can overcome the problems of large anisotropy of general fibre reinforced material and fibre-floating on the surface of product.
Aiming at the defects of nylon and polyphenyl ether, the invention adopts the potassium titanate whisker to be matched with other raw materials, and provides the nylon polyphenyl ether composite material which has the advantages of wear resistance, high strength, high temperature resistance, low water absorption, stable size and organic solvent resistance.
The technical scheme is as follows:
a nylon polyphenylene oxide composite material comprises the following components in percentage by mass:
the diameter of the potassium titanate whisker is 0.1-2 mu m, and the length is 1-100 mu m;
the particle size of the polytetrafluoroethylene micro powder is less than 200 mu m, and the D50 particle size is less than 40 mu m.
The nylon polyphenyl ether composite material disclosed by the invention is prepared by compounding nylon and polyphenyl ether, and adopting the compatilizer, the potassium titanate whisker and the polytetrafluoroethylene micropowder in a matching manner, so that the performance defects of each single resin can be obviously improved, and the alloy material with excellent and balanced performances such as wear resistance, mechanical property, processability, temperature resistance, chemical resistance, hydrolysis resistance, dimensional stability and the like is obtained. Furthermore, the potassium titanate whisker and the polytetrafluoroethylene micro powder reinforced filling material are matched, so that the appearance of the material which is better than the conventional glass fiber, carbon fiber and mineral powder filled and reinforced material can be obtained, the glossiness is higher, the wear resistance is better, the size stability is better, and the application fields of nylon and polyphenyl ether materials are greatly widened.
In the present invention, the nylon polyphenylene ether composite material comprises 5 to 50% by mass of potassium titanate whiskers, including but not limited to 5%, 10%, 12%, 15%, 20%, 25%, 30%, 35%, 40%, 45% and 50%, preferably 10 to 40%.
In the invention, the potassium titanate whisker has the diameter of 0.1-2 μm and the length of 1-100 μm; preferably, the potassium titanate whisker has a diameter of 0.1 to 1 μm and a length of 10 to 20 μm.
In one embodiment, the chemical composition of the potassium titanate whisker is K 2 O·2TiO 2 、K 2 O·4TiO 2 、K 2 O·6TiO 2 、K 2 O·8TiO 2 Preferably K 2 O·6TiO 2 Or K 2 O·8TiO 2 。
In one embodiment, the potassium titanate whiskers are NP-TW2 of Shanghai peak pelargonium whiskers, have a diameter of 0.1 μm to 2 μm, and have a length of 1 μm to 100 μm.
In one embodiment, the potassium titanate whiskers are TISMO-N from tsukamur kanji whiskers in japan, and have a diameter of 0.1 μm to 1 μm and a length of 10 μm to 20 μm.
In the present invention, the nylon polyphenylene ether composite material further comprises 20% to 60% by mass of nylon resin, including but not limited to 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55% and 60%, preferably 22% to 55%.
In one embodiment, the nylon resin is selected from semi-crystalline nylons having a melting point of aliphatic and/or semi-aromatic.
In one embodiment, the nylon resin is selected from the group consisting of polycaprolactam, polytetramethylene adipamide, polypentamethyleneadipamide, polyhexamethylene adipamide, polyhexamethylene sebacamide, polyhexamethylene dodecacarbodiimide, polyundecanolactam, polydodecanolactam, polydodecanodidodecadiamine, copolynylhexamethylene terephthalamide/isophthalamide, copolynylnylon of polyhexamethylene terephthalamide/hexamethylene adipamide, copolynylnylon of polyhexamethylene terephthalamide/hexamethylene isophthalamide/hexamethylene adipamide, copolynylnylon of polyhexamethylene terephthalamide/caprolactam, copolynylnylon of polyhexamethylene terephthalamide/2-methylpentamethylene terephthalamide, polyparanonanediamide terephthalamide, and polyparadecanediamideOne or a mixture of several of them. Further preferably, at least one aliphatic semi-crystalline nylon (having a melting point T of m 210 ℃ to 270 ℃) and/or semi-aromatic semi-crystalline nylons (melting point T thereof) m At 270-340 deg.c.
In one embodiment, the nylon resin is PA66 EPR24 (melting point 252 ℃) from the Henan deity horse group, PA612 (melting point 217 ℃) from DuPont, USA, or PPA N600 (melting point 308 ℃) from New and adults, inc., hejiang.
In the present invention, the nylon polyphenylene ether composite material further comprises 10% to 50% of polyphenylene ether resin by mass, including but not limited to 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% and 50%, preferably 15% to 30%.
In one embodiment, the polyphenylene ether resin has a Ubbelohde intrinsic viscosity of 0.2dl/g to 0.8dl/g, including but not limited to 0.2dl/g, 0.3dl/g, 0.4dl/g, 0.45dl/g, 0.5dl/g, 0.6dl/g, 0.7dl/g, and 0.8dl/g, preferably 0.4dl/g to 0.6dl/g, in chloroform at 25 ℃.
In one embodiment, the polyphenylene ether resin is LXR045 available from Ranunculus sieboldii chemical, and the intrinsic viscosity of the resin is 0.45dl/g as measured by a Ubbelohde viscometer at 25 ℃ in chloroform.
In the invention, the nylon polyphenylene oxide composite material also comprises 3-10% of compatilizer by mass percent, including but not limited to 2%, 3%, 5%, 6%, 7%, 8%, 9% and 10%, preferably 3-8%.
In one embodiment, the compatibilizer is a maleic anhydride grafted polymer having a grafting ratio of 0.5% to 5.0%. It is understood that the graft ratio of the maleic anhydride graft polymer is 0.5% to 5.0%, including but not limited to: 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.2%, 1.4%, 1.5%, 1.6%, 1.8%, 2.0%, 2.2%, 2.5%, 2.8%, 3.0%, 3.2%, 3.5%, 3.6%, 3.8%, 4.0%, 4.2%, 4.4%, 4.5%, 4.6%, 4.8%, 5.0%. Preferably, the grafting rate of the maleic anhydride grafted polymer is 0.5-3%, so that the good compatibility of a nylon polyphenylene oxide composite system can be ensured, and the problem of layering caused by incompatibility of two resins can be effectively solved.
In one embodiment, the maleic anhydride grafted polymer is selected from one or more of maleic anhydride grafted polyolefin elastomer (POE-g-MAH), maleic anhydride grafted hydrogenated styrene-butadiene block copolymer (SEBS-g-MAH) and maleic anhydride grafted polyphenylene oxide (PPO-g-MAH).
The polytetrafluoroethylene, commonly known as plastic king, has a melting point of 325-335 ℃, and has excellent chemical stability, corrosion resistance, sealing property, high lubrication non-sticking property, electrical insulation property and good ageing resistance. According to the invention, the polytetrafluoroethylene micro powder and the potassium titanate whisker are compounded to serve as the reinforced filling material, so that the appearance of the material which is better than that of the conventional glass fiber, carbon fiber and mineral powder filled and reinforced material can be obtained, the glossiness of the material is higher, the wear resistance of the material is better, the size stability of the material is better, and the application fields of nylon and polyphenyl ether materials are greatly expanded.
In the present invention, the nylon polyphenylene ether composite material comprises 5% to 20% by mass of polytetrafluoroethylene fine powder, including but not limited to 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 15%, 16%, 17%, 18%, 19% and 20%, preferably 10% to 18%.
In the invention, the particle size of the polytetrafluoroethylene micro powder is less than 200 mu m, and the D50 particle size is less than 40 mu m.
In one embodiment, the particle size of the polytetrafluoroethylene micro powder is 10-200 μm, and the D50 particle size is 20-30 μm.
In one embodiment, the polytetrafluoroethylene micropowder is KTL-630 from Xiduocun, japan, and has a D50 particle size of 20 to 30 μm.
In one embodiment, the nylon polyphenylene ether composite material comprises the following components in percentage by weight:
in one embodiment, the nylon polyphenylene oxide composite material further comprises one or more of an antioxidant, a lubricant, a nucleating agent and a coupling agent. Wherein the antioxidant can enhance the stability of the composite material. The lubricant can perform the functions of lubrication, improvement of dispersibility and mold release. The nucleating agent enables the mechanical property, the heat resistance and the dimensional stability of the material to be more excellent. The coupling agent is beneficial to enhancing the wettability and the dispersibility between the inorganic material and the organic material, can greatly improve the bending strength, the tensile strength and the interlaminar shear strength of the produced composite material, and obviously improves the wet electrical performance.
In one embodiment, the nylon polyphenylene ether composite further comprises 0.2% to 0.5% of an antioxidant, including but not limited to 0.2%, 0.3%, 0.4% and 0.5%, preferably 0.2% to 0.4%.
In one embodiment, the antioxidant is selected from N, N' -1, 6-hexylene-bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionamide](an antioxidant 1098),
S9228, tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid]Pentaerythritol ester, N' -bis- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-dicumylphenyl) pentaerythritol diphosphite, potassium iodide and cuprous iodide. Preferably, the antioxidant is antioxidant 1098 and->
S9228, antioxidant 1098 and/or->
The mass ratio of S9228 is 1: (0.1-5). />
In one embodiment, the nylon polyphenylene ether composite further comprises an anti-lubricant agent 0.1% to 0.5%, including but not limited to 0.1%, 0.2%, 0.3%, 0.4% and 0.5%, preferably 0.2% to 0.5%.
In one embodiment, the lubricant is one or more of calcium stearate, N' -ethylene bis stearamide, ethylene acrylic acid copolymer, OP wax and E wax.
In one embodiment, the lubricant is an OP wax.
In one embodiment, the nylon polyphenylene ether composite further comprises 0.1% to 1% of a nucleating agent, including but not limited to 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9% and 1%, preferably 0.2% to 0.8%.
In one embodiment, the nucleating agent is selected from one or more of long-carbon-chain calcium carboxylate nucleating agents, substituted aryl heterocyclic phosphate nucleating agents, aryl aluminum carboxylate nucleating agents and aromatic amide nucleating agents.
In one embodiment, the nucleating agent is CAV102 of Craine.
In one embodiment, the nylon polyphenylene ether composite further comprises 0.1-1% of a coupling agent including, but not limited to, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, and 1%, preferably 0.2-0.8%.
In one embodiment, the coupling agent is an amino silane coupling agent. The amino silane coupling agent is beneficial to enhancing the wettability and the dispersibility between an inorganic material and an organic material, can greatly improve the bending strength, the tensile strength and the interlaminar shear strength of a produced composite material, and obviously improves the wet electrical performance, and the bending strength and the tensile strength of the composite material are improved before and after soaking.
In one embodiment, the coupling agent is selected from one or more of KH550, KH560 and KH 570.
In one embodiment, the nylon polyphenylene oxide composite material comprises the following components in percentage by mass:
in one embodiment, the nylon polyphenylene oxide composite material comprises the following components in percentage by mass:
the invention also provides a preparation method of the nylon polyphenylene oxide composite material, which comprises the following steps:
and mixing, melting and extruding the nylon resin, the polyphenyl ether resin, the compatilizer, the potassium titanate whisker and the polytetrafluoroethylene micro powder.
In one embodiment, the preparation method of the nylon polyphenylene oxide composite material comprises the following steps:
mixing the nylon resin, the polyphenyl ether resin, the compatilizer, the polytetrafluoroethylene micro powder, the antioxidant, the lubricant and the nucleating agent to obtain a mixture I;
stirring and mixing the coupling agent hydrolyzed in advance and the potassium titanate whisker at a high speed, and then placing the mixture in an oven at 100-120 ℃ for drying for 2-3 hours to obtain a mixture II;
and mixing the mixture I and the mixture II, melting, extruding and granulating.
In one embodiment, the melt extrusion is carried out by a double-screw extruder, and the length-diameter ratio of screws of the double-screw extruder is (44-48): 1, the rotating speed of a screw is 200-400 rpm, a charging barrel of the double-screw extruder is ten-section barrel, the first section of barrel is connected with a main feeding device, the fourth section of barrel is exhausted, the sixth section of barrel is connected with a side feeding device, and the ninth section of barrel is vacuumized; the barrel temperature is set as: 220 +/-60 ℃ of a first section of cylinder body, 240 +/-60 ℃ of a second section of cylinder body, 250 +/-60 ℃ of a third section of cylinder body, 260 +/-60 ℃ of a fourth section of cylinder body, 260 +/-60 ℃ of a fifth section of cylinder body, 270 +/-60 ℃ of a sixth section of cylinder body, 270 +/-60 ℃ of a seventh section of cylinder body, 270 +/-60 ℃ of an eighth section of cylinder body, 270 +/-60 ℃ of a ninth section of cylinder body, 270 +/-60 ℃ of a tenth section of cylinder body and 280 +/-60 ℃ of a machine head.
The invention also provides application of the nylon polyphenylene oxide composite material. The technical scheme is as follows:
an electronic appliance comprising the nylon polyphenylene ether composite material as described above.
An automobile comprising a nylon polyphenylene ether composite as described above.
The following are specific examples, and the main raw materials of the present invention are as follows:
the proportions and percentages of the components of the examples are based on mass, and the components are as follows:
a is PA resin:
a1: PA66 EPR24, melting point 252 ℃, available from the Henan Shenma group;
a2: PA612, melting point 217 ℃, available from DuPont, USA;
a3: PPAN600, melting point 308 ℃, zhejiang New Yongji Co., ltd;
b is PPO resin:
LXR045, intrinsic viscosity 0.45dl/g, purchased from Ranunculus sieboldii chemical industry;
c is a compatilizer:
c1: PPO-g-MAH, GPM-450C MAH grafting rate 3%, purchased from Ningwave energy light;
c2: POE-g-MAH, CMG-5805MAH grafting rate is 0.5% -1%, and the POE-g-MAH is easy to purchase in Shanghai;
d is potassium titanate whisker:
d1: TISMO-N with the diameter of 0.1-1 μm and the length of 10-20 μm is purchased from Tsukamur japonica;
d2: NP-TW2, diameter is 0.1 μm-2 μm, length is 1 μm-100 μm, purchase in Shanghai Peak Zhu whisker;
e is polytetrafluoroethylene micro powder:
KTL-630 (E1: KTL-630) with D50 particle size of 20-30 μm, available in Xiduocun, japan;
FA-500H as E2, with the D50 particle size of 400-800 μm, and large gold fluoride;
f is an antioxidant:
antioxidant 1098 and
s9228 is prepared by compounding according to the mass ratio of 1;
g is a lubricant:
OP wax
H is a nucleating agent:
CAV102, available from Kelaien;
i is a coupling agent:
KH550；
j is alkali-free chopped glass fiber:
ECS11-3-568H, 11 μm in diameter, purchased from megalite group;
examples 1 to 5 and comparative examples 1 to 6 were weighed and compounded according to table 2, and PA resin, PPO resin, a compatibilizer, polytetrafluoroethylene fine powder, an antioxidant, a lubricant, and a nucleating agent were mixed to obtain a mixture I; stirring and mixing the coupling agent hydrolyzed in advance and the potassium titanate whisker at a high speed, and then drying in an oven at 120 ℃ for 2-3 hours to obtain a mixture II; and finally, respectively putting the mixture I and the mixture II into a main feeding hopper and a side feeding hopper, and performing melt extrusion and granulation by a double-screw extruder according to a proportion. Specifically, the cartridge temperatures of example 1, example 2, example 3, comparative example 1, comparative example 2, comparative example 3, and comparative example 6 were set to: 220 +/-5 ℃ of a first cylinder, 240 +/-5 ℃ of a second cylinder, 250 +/-5 ℃ of a third cylinder, 260 +/-5 ℃ of a fourth cylinder, 260 +/-5 ℃ of a fifth cylinder, 270 +/-5 ℃ of a sixth cylinder, 270 +/-5 ℃ of a seventh cylinder, 270 +/-5 ℃ of an eighth cylinder, 270 +/-5 ℃ of a ninth cylinder, 270 +/-5 ℃ of a tenth cylinder and 280 +/-5 ℃ of a head; the barrel temperatures of example 4, example 5, comparative example 4 and comparative example 5 were set as follows: 260 +/-5 ℃ of a first section of cylinder body, 280 +/-5 ℃ of a second section of cylinder body, 300 +/-5 ℃ of a third section of cylinder body, 300 +/-5 ℃ of a fourth section of cylinder body, 300 +/-5 ℃ of a fifth section of cylinder body, 310 +/-5 ℃ of a sixth section of cylinder body, 310 +/-5 ℃ of a seventh section of cylinder body, 310 +/-5 ℃ of an eighth section of cylinder body, 310 +/-5 ℃ of a ninth section of cylinder body, 310 +/-5 ℃ of a tenth section of cylinder body and 320 +/-5 ℃ of a head.
TABLE 1
The PA/PPO composite materials prepared in examples 1-5 and comparative examples 1-6 were subjected to mechanical property correlation tests according to the national standard injection molding standard test bars.
The notched impact test was carried out with reference to the national standard GB/T1843.
The tensile test is carried out according to the national standard GB/T1040.
The bending test is carried out with reference to the national standard GB/T9341.
The thermal deformation (1.80 MPa/4.0 mm) test is carried out with reference to the national standard GB/T1634.
The friction coefficient test was carried out with reference to GB/T10006-2021.
Gloss: the glossiness test is carried out according to the national standard GB/T9754.
Chemical resistance: and (3) applying stress to the sample strip by a self-made clamp to prepare the GB standard tensile sample strip through injection molding, and soaking the sample strip in glacial acetic acid to carry out organic solvent resistance test.
The test results of examples 1 to 5 and comparative examples 1 to 6 are shown in Table 2.
TABLE 2
As can be seen from Table 2, the composite materials provided by the embodiments 1-5 of the invention have good wear resistance, high temperature resistance, glossiness, mechanical strength, chemical resistance and dimensional stability, are suitable for injection molding processing technology, and meet the requirements of wear-resistant parts with high precision requirements.
It can be seen from the comparison between example 1 and comparative example 1 that the shrinkage and water absorption of the composite material are both significantly increased by omitting the addition of PPO. It can be seen from the comparison between example 2 and comparative example 2 that the composite material has poor mechanical strength, heat resistance, wear resistance (coefficient of friction), shrinkage and other properties although the composite material has good glossiness and low abrasion without adding the potassium titanate whisker for reinforcement. It can be seen from comparison of example 2 and comparative example 3 that the addition of the PTFE fine powder is omitted, and the abrasion resistance of the composite material is poor, particularly the amount of abrasion is significantly increased. It can be seen from the comparison between example 4 and comparative example 4 that the potassium titanate whiskers were replaced by the same amount of glass fibers, and although the mechanical properties of the composite material were not greatly different, the abrasion resistance, gloss and shrinkage (in the vertical direction) were significantly inferior. It can be seen from comparison of example 4 and comparative example 5 that the abrasion resistance and gloss of the composite material are significantly poor by using the PTFE micropowder having a coarser particle size. It can be seen from the comparison of example 1 and comparative example 6 that the chemical resistance of the composite material is poor without the addition of nylon.
FIG. 1 is a graph showing the effect of the nylon polyphenylene ether composite material prepared in comparative example 3 after a friction test (with a deep grinding mark); FIG. 2 is a graph showing the effect of the nylon polyphenylene ether composite obtained in example 2 after a friction test (wear scar is very light). Comparing fig. 1 and fig. 2, it can be known that adding PTFE micropowder can effectively reduce abrasion and improve wear resistance of the material.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (14)
1. The nylon polyphenylene oxide composite material is characterized by comprising the following components in percentage by mass:
the diameter of the potassium titanate whisker is 0.1-2 mu m, and the length is 1-100 mu m;
the particle size of the polytetrafluoroethylene micro powder is less than 200 mu m, and the particle size of D50 is less than 40 mu m.
2. The nylon polyphenylene ether composite material according to claim 1, wherein the potassium titanate whiskers have a diameter of 0.1 to 1 μm and a length of 10 to 20 μm.
3. The nylon polyphenylene ether composite material as claimed in claim 1, wherein the chemical composition of the potassium titanate whisker is K 2 O·2TiO 2 、K 2 O·4TiO 2 、K 2 O·6TiO 2 And K 2 O·8TiO 2 One or more of them.
4. The nylon polyphenylene ether composite material according to claim 1, wherein the polyphenylene ether resin has an intrinsic Ubbelohde viscosity of 0.2dl/g to 0.8dl/g in chloroform at 25 ℃.
5. The nylon polyphenylene ether composite material according to claim 1, wherein the compatibilizer is a maleic anhydride graft polymer having a graft ratio of 0.5% to 5.0%.
6. The nylon polyphenylene ether composite material according to claim 5, wherein the maleic anhydride grafted polymer is one or a mixture of maleic anhydride grafted polyolefin elastomer, maleic anhydride grafted hydrogenated styrene-butadiene block copolymer and maleic anhydride grafted polyphenylene ether.
7. The nylon polyphenylene ether composite material according to any one of claims 1 to 6, wherein the nylon resin is selected from semi-crystalline nylons having a melting point of aliphatic and/or semi-aromatic.
8. The nylon-polyphenylene ether composite material according to claim 7, wherein the nylon resin is selected from the group consisting of polycaprolactam, polytetramethylene adipamide, polypentylglycol adipamide, polyhexamethylene sebacamide, polyhexamethylene dodecadicarboxamide, polydecamethylene dodecacarboxamide, polyundecanolactam, polydodecanolactam, polydodecanoyldodecadiamine, a copolymerized nylon of polyhexamethylene terephthalamide/m-hexamethylene terephthalamide, a copolymerized nylon of polyhexamethylene terephthalamide/hexamethylene adipamide, a copolymerized nylon of polyhexamethylene terephthalamide/m-hexamethylene isophthalamide/hexamethylene adipamide, a copolymerized nylon of polyhexamethylene terephthalamide/caprolactam, a copolymerized nylon of polyhexamethylene terephthalamide/2-methylpentamethylene terephthalamide, a copolymerized nylon of polynaphthalenediamide and polydecamethylene terephthalamide.
9. The nylon polyphenylene ether composite material according to claim 7, further comprising one or more of an antioxidant, a lubricant, a nucleating agent and a coupling agent.
10. The nylon polyphenylene ether composite material according to claim 9, further comprising an antioxidant in an amount of 0.2 to 0.5% by mass; 0.1 to 0.5 percent of lubricant; 0.1 to 1 percent of nucleating agent; and 0.1 to 1 percent of coupling agent.
11. The nylon polyphenylene ether composite material according to claim 10, wherein the antioxidant is selected from the group consisting of N, N' -1, 6-hexylene-bis [3- (3, 5-di-t-butyl-4-hydroxyphenyl) propionamide]、
S9228, tetrakis [ beta- (3, 5-di-tert-butyl)Butyl-4-hydroxyphenyl) propionic acid]One or a mixture of more of pentaerythritol ester, N' -bis- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-dicumylphenyl) pentaerythritol diphosphite, potassium iodide and cuprous iodide; and/or
The lubricant is one or a mixture of more of calcium stearate, N' -ethylene bis stearamide, ethylene acrylic acid copolymer, OP wax and E wax; and/or
The nucleating agent is selected from one or a mixture of more of long-carbon-chain calcium carboxylate nucleating agent, substituted aryl heterocyclic phosphate nucleating agent, aryl aluminum carboxylate nucleating agent and aromatic amide nucleating agent; and/or
The coupling agent is an amino silane coupling agent.
12. A method for preparing a nylon polyphenylene ether composite material according to any one of claims 1 to 11, comprising the steps of:
and mixing, melting and extruding the nylon resin, the polyphenyl ether resin, the compatilizer, the potassium titanate whisker and the polytetrafluoroethylene micro powder.
13. An electronic appliance comprising the nylon polyphenylene ether composite material according to any one of claims 1 to 11.
14. An automobile comprising the nylon polyphenylene ether composite material according to any one of claims 1 to 11.
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