CN109627684B - Ternary alloy containing aromatic polyamide and preparation method thereof - Google Patents
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Abstract
The invention relates to the technical field of high polymer materials, in particular to a ternary alloy containing aromatic polyamide and a preparation method thereof, and the ternary alloy containing aromatic polyamide is prepared from the following raw materials in parts by weight: 70-94 parts of polyether-ether-ketone, 3-20 parts of polyetherimide and 3-10 parts of aromatic polyamide; the aromatic polyamide is aromatic polyamide containing an ether ketone structure or aromatic polyamide containing naphthalene; according to the records of the embodiment, the friction coefficient of the ternary alloy is reduced by more than or equal to 4.7 percent compared with the friction coefficient of pure-phase PEEK, the wear rate is reduced by more than or equal to 35.3 percent, and the mechanical property of the ternary alloy is greatly improved compared with that of the pure-phase PEEK.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a ternary alloy containing aromatic polyamide and a preparation method thereof.
Background
polyether ether ketone (PEEK) is a special engineering plastic with excellent comprehensive performance. As a semi-crystalline thermoplastic polymer material, the flame retardant thermoplastic polymer material has excellent flame retardance, radiation resistance, high temperature resistance and mechanical properties. Meanwhile, in the aspect of frictional wear performance, the polyetheretherketone is a good friction-reducing wear-resisting material after Polytetrafluoroethylene (PTFE). Therefore, the method is widely applied to the fields of aerospace, instruments and meters, automobile industry and the like.
Aromatic Polyamides (PK) were first developed by dupont in 1967, have good high temperature resistance, chemical resistance and fatigue resistance, and have excellent friction resistance. At present, the composite material is widely applied to tire and fuselage materials of airplanes, and some structural parts of rockets and artificial satellites are also made of composite materials reinforced by poly (p-phenylene terephthalamide) (PPTA) fibers, so that the quality of flight related instruments is greatly reduced, and the economic cost is saved.
blending is an important method for developing new materials, excellent comprehensive performance can be obtained, and the method has the advantage of low cost compared with the introduction of new groups on a main chain structure and copolymerization. If the aromatic polyamide can be introduced into a polyether-ether-ketone system, the processing of the aromatic polyamide can be realized, and the friction and mechanical properties of polyether-ether-ketone can be improved.
however, the melting temperature of the aromatic polyamide exceeds the decomposition temperature due to strong hydrogen bond interaction between chains of the aromatic polyamide, and the post-processing process has great difficulty. And the higher crystallinity also makes the material have weak dissolving capacity and can only be dissolved in concentrated sulfuric acid generally. These disadvantages greatly limit the range of applications of aromatic polyamides in blended materials.
Disclosure of Invention
The invention aims to provide a ternary alloy containing aromatic polyamide and a preparation method thereof, wherein polyether imide (PEI) can uniformly disperse PK in a PEEK matrix, and the mechanical and frictional properties of the ternary alloy are improved.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a ternary alloy containing aromatic polyamide, which is prepared from the following raw materials in parts by weight:
70-94 parts of polyether-ether-ketone
3-20 parts of polyetherimide
3-10 parts of aromatic polyamide;
The aromatic polyamide is aromatic polyamide containing an ether ketone structure or aromatic polyamide containing naphthalene.
Preferably, the reduced viscosity of the polyether-ether-ketone is 0.8-1.0 dL/g, and the glass transition temperature is 142-144 ℃.
Preferably, the polyetherimide has a reduced viscosity of 0.4-0.6 dL/g and a glass transition temperature of 215-217 ℃.
Preferably, the aromatic polyamide has a reduced viscosity of 0.4-1.0 dL/g;
When the aromatic polyamide is aromatic polyamide containing an ether ketone structure, the glass transition temperature of the aromatic polyamide containing the ether ketone structure is 325-328 ℃;
When the aromatic polyamide is a naphthalene-containing aromatic polyamide, the glass transition temperature of the naphthalene-containing aromatic polyamide is 285-288 ℃.
The invention also provides a preparation method of the ternary alloy containing the aromatic polyamide, which comprises the following steps:
Mixing aromatic polyamide, polyetherimide, cosolvent and organic solvent, and discharging in deionized water to obtain a binary blend of aromatic polyamide/polyetherimide;
and mixing the binary blend of the aromatic polyamide/polyetherimide with the polyether-ether-ketone, and sequentially performing extrusion, granulation, injection molding and annealing to obtain the ternary alloy containing the aromatic polyamide.
Preferably, the cosolvent is one or more of calcium chloride, lithium chloride, magnesium chloride and methyl tri-n-butyl ammonium chloride;
The organic solvent is one or more of N, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and hexamethylphosphoramide.
Preferably, the extrusion is carried out in a double-screw extruder, the extrusion temperature is 360-390 ℃, and the rotating speed of the double-screw extruder is 20-60 r/min.
Preferably, the injection molding temperature is 380-400 ℃, and the injection molding pressure is 700-900 bar.
preferably, the annealing temperature is 200-210 ℃, and the annealing time is 3-5 hours.
The invention provides a ternary alloy containing aromatic polyamide, which is prepared from the following raw materials in parts by weight: 70-94 parts of polyether-ether-ketone, 3-20 parts of polyetherimide and 3-10 parts of aromatic polyamide; the aromatic polyamide is aromatic polyamide containing an ether ketone structure or aromatic polyamide containing naphthalene; PEI and PEEK have good thermodynamic compatibility, a binary blend of aromatic polyamide and polyether imide can be added into polyether ether ketone, and the aromatic polyamide is uniformly dispersed in a PEEK matrix under the medium action of PEI, so that the processing of the aromatic polyamide is realized, and compared with PEEK pure phase, the mechanical and frictional properties of the ternary alloy are improved. According to the records of the embodiment, the friction coefficient of the ternary alloy is reduced by more than or equal to 4.7 percent compared with the friction coefficient of pure-phase PEEK, the wear rate is reduced by more than or equal to 35.3 percent, and the mechanical property of the ternary alloy is greatly improved compared with that of the pure-phase PEEK.
Detailed Description
the invention provides a ternary alloy containing aromatic polyamide, which is prepared from the following raw materials in parts by weight:
70-94 parts of polyether-ether-ketone
3-20 parts of polyetherimide
3-10 parts of aromatic polyamide;
The aromatic polyamide is aromatic polyamide containing an ether ketone structure or aromatic polyamide containing naphthalene.
In the present invention, the starting components are all commercially available products well known to those skilled in the art unless otherwise specified.
According to the weight parts, the preparation raw material of the ternary alloy containing the aromatic polyamide comprises 70-94 parts of polyether-ether-ketone, preferably 75-90 parts, and more preferably 85-90 parts. In the invention, the reduced viscosity of the polyether-ether-ketone is preferably 0.8-1.0 dL/g, and more preferably 0.85-0.95 dL/g; the glass transition temperature of the polyether-ether-ketone is preferably 142-144 ℃.
the preparation raw material of the ternary alloy containing the aromatic polyamide comprises, by weight, 3-20 parts of polyetherimide, preferably 5-15 parts, and more preferably 8-10 parts. In the invention, the reduced viscosity of the polyetherimide is preferably 0.4-0.6 dL/g, and more preferably 0.45-0.55 dL/g; the glass transition temperature of the polyetherimide is preferably 215-217 ℃.
The preparation raw material of the ternary alloy containing the aromatic polyamide comprises 3-10 parts by weight of the aromatic polyamide, preferably 4-9 parts by weight, and more preferably 5-8 parts by weight. In the invention, the aromatic polyamide reduced viscosity is preferably 0.4-1.0 dL/g, more preferably 0.5-0.8 dL/g, and most preferably 0.5-0.6 dL/g;
When the aromatic polyamide is aromatic polyamide containing an ether ketone structure, the glass transition temperature of the aromatic polyamide containing the ether ketone structure is preferably 325-328 ℃;
When the aromatic polyamide is a naphthalene-containing aromatic polyamide, the glass transition temperature of the naphthalene-containing aromatic polyamide is preferably 285-288 ℃.
In the invention, the aromatic polyamide is aromatic polyamide (PK-1) containing ether ketone structure or aromatic polyamide (PK-2) containing naphthalene; in the present invention, the kind and the preparation method of the aromatic polyamide containing an etherketone structure are preferably the kind and the preparation method of the aromatic polyamide containing an etherketone structure disclosed in application No. CN 103524730A.
In the present invention, the aromatic polyamide is a method for producing a naphthalene-containing aromatic polyamide, preferably comprising the steps of: mixing 1, 5-naphthalene diamine and 4,4' -diphenyl ether diacyl chloride in a molar ratio of 1:1, taking NMP as a solvent and LiCl as a catalyst to perform polymerization reaction at room temperature; the amounts of NMP and LiCl used in the present invention are not particularly limited, and those known to those skilled in the art may be used. In the present invention, the structural formula of the naphthalene-containing aromatic polyamide is preferably:
The invention does not have any special limitation on n in the structural formula, and the naphthalene-containing aromatic polyamide can have the reduced viscosity of 0.4-1.0 dL/g and the glass transition temperature of 285-288 ℃.
the invention also provides a preparation method of the ternary alloy containing the aromatic polyamide, which comprises the following steps:
Mixing aromatic polyamide, polyetherimide, cosolvent and organic solvent, and discharging in deionized water to obtain a binary blend of aromatic polyamide/polyetherimide;
And mixing the binary blend of the aromatic polyamide/polyetherimide with the polyether-ether-ketone, and sequentially performing extrusion, granulation, injection molding and annealing to obtain the ternary alloy containing the aromatic polyamide.
the method comprises the steps of mixing aromatic polyamide, polyetherimide, cosolvent and organic solvent, and discharging in deionized water to obtain the binary blend of aromatic polyamide/polyetherimide. In the invention, the cosolvent is preferably one or more of calcium chloride, lithium chloride, magnesium chloride and methyl tri-n-butyl ammonium chloride; when the cosolvent is more than two of the specific choices, the proportion of the specific substances is not limited in any way, and the specific substances can be mixed according to any proportion.
In the invention, the organic solvent is preferably one or more of N, N-dimethylacetamide (DMAc), N-methylpyrrolidone (NMP), N, N-Dimethylformamide (DMF) and hexamethylphosphoramide; when the organic solvent is more than two of the above specific choices, the invention has no special limitation on the proportion of the specific substances, and the specific substances can be mixed according to any proportion.
In the present invention, the mass ratio of PK to co-solvent is preferably 1: (0.1-2), more preferably 1: (0.5 to 1.5), most preferably 1: (0.8 to 1.2); in the present invention, the mass ratio of the total mass of PK and PEI to the organic solvent is preferably 1: (5-10), more preferably 1: (6-8).
In the present invention, the mixing is preferably performed under stirring; the stirring is not particularly limited in the present invention, and a stirring process known to those skilled in the art may be employed.
The amount of the deionized water used in the present invention is not particularly limited, and may be an amount well known to those skilled in the art to precipitate the crude aromatic polyamide/polyetherimide blend from the organic solvent.
After the discharging is finished, the crude product obtained by discharging is preferably crushed, washed by boiled deionized water and absolute ethyl alcohol in sequence, repeated for 2-5 times and dried to obtain a binary blend of aromatic polyamide/polyetherimide; the invention has no special limitation on the crushing process, and the crushing process known by the technicians in the field can be adopted; the present invention does not have any particular limitation on the drying process, and a drying process known to those skilled in the art may be adopted.
In the invention, the PEI has good solubility in the organic solvent, and the molecular chain of the PEI and the molecular chain of the PK can be intertwined by the mixing, so that the aim of uniformly mixing the PK and the PEI is fulfilled. Meanwhile, PEI and PEEK have good thermodynamic compatibility, and the polyaramid can be better dispersed in a PEEK matrix in the follow-up process.
after the binary blend of the aromatic polyamide/polyetherimide is obtained, the binary blend of the aromatic polyamide/polyetherimide and polyether-ether-ketone are mixed, and then extrusion granulation, injection molding and annealing are sequentially carried out to obtain the ternary alloy containing the aromatic polyamide. In the present invention, the mixing is preferably performed under stirring conditions, and the stirring is not particularly limited in the present invention, and may be performed by a stirring process well known to those skilled in the art.
after completion of the stirring, the present invention preferably dries the resulting mixture. In the present invention, the drying is preferably vacuum drying; the temperature of the vacuum drying is preferably 80-120 ℃, and more preferably 90-110 ℃; the vacuum drying time is preferably 5 to 12 hours, and more preferably 8 to 10 hours.
In the invention, the extrusion is preferably carried out in a double-screw extruder, and the extrusion temperature is preferably 360-390 ℃, more preferably 365-385 ℃, and most preferably 370-380 ℃; the rotating speed of the double-screw extruder is preferably 20-60 r/min, and more preferably 30-50 r/min. In the present invention, the granulation is preferably carried out in a granulator; the granulation conditions of the present invention are not particularly limited, and may be those known to those skilled in the art.
After the extrusion and granulation are finished, the extruded and granulated product is preferably dried and then subjected to injection molding. In the present invention, the drying is preferably vacuum drying; the temperature of the vacuum drying is preferably 80-120 ℃, more preferably 90-110 ℃, and most preferably 95-105 ℃; the vacuum drying time is preferably 5 to 12 hours, and more preferably 8 to 10 hours.
In the invention, the injection molding temperature is preferably 380-400 ℃, more preferably 385-395 ℃, and most preferably 388-392 ℃; the pressure of the injection molding is preferably 700-900 bar, and more preferably 750-850 bar.
In the invention, the annealing temperature is preferably 200-210 ℃, more preferably 202-208 ℃, and most preferably 204-206 ℃; the annealing time is preferably 3 to 5 hours, and more preferably 3.5 to 4.5 hours.
In the present invention, the annealing may promote complete crystallization of the ternary alloy.
the ternary alloy containing aromatic polyamide and the preparation method and application thereof provided by the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
example 1
Mixing 6g of PK-1 powder, 6g of PEI powder, 1g of LiCl and 60mLNMP, dissolving under stirring, discharging in deionized water, crushing a crude product, washing with boiled deionized water and absolute ethyl alcohol for 3 times respectively, and drying to obtain a powdery PK-1/PEI binary blend;
mixing 94g of PEEK powder and 6g of PK-1/PEI binary blend powder, adding the mixture into a high-speed stirrer, uniformly mixing the mixture at a high speed for 10min, putting the mixture into a vacuum oven to dry the mixture for 8 hours at 100 ℃, adding the dried mixture into a double-screw extruder, extruding the mixture at the temperature of 370 ℃ and the screw rotating speed of 40r/min, granulating, and drying the mixture for 12 hours at 120 ℃ in vacuum to obtain PEEK/PEI/PK-1 ternary alloy granules;
and (3) carrying out injection molding on the PEEK/PEI/PK-1 ternary alloy granules at 380 ℃ and 750bar, and then annealing for 4 hours at 210 ℃ to obtain the PEEK/PEI/PK-1 ternary alloy.
example 2
Mixing 10g of PK-1 powder, 10g of PEI powder, 2g of LiCl and 150ml of LNMP, dissolving under stirring, discharging in deionized water, crushing a crude product, washing with boiled deionized water and absolute ethyl alcohol for 3 times respectively, and drying to obtain a powdery PK-1/PEI binary blend;
Mixing 90g of PEEK powder and 10g of PK-1/PEI binary blend powder, adding the mixture into a high-speed stirrer, uniformly mixing the mixture at a high speed for 10min, putting the mixture into a vacuum oven to dry the mixture for 8 hours at 100 ℃, adding the dried mixture into a double-screw extruder, extruding the mixture at the temperature of 380 ℃ and the screw rotating speed of 40r/min, granulating, and drying the mixture for 12 hours at the temperature of 120 ℃ in vacuum to obtain PEEK/PEI/PK-1 ternary alloy granules;
And (3) carrying out injection molding on the PEEK/PEI/PK-1 ternary alloy granules at the temperature of 400 ℃ and at the bar of 900bar, and then annealing for 5 hours at the temperature of 200 ℃ to obtain the PEEK/PEI/PK-1 ternary alloy.
Example 3
Mixing 15g of PK-1 powder, 15g of PEI powder, 5g of LiCl and 300mLNMP, dissolving under stirring, discharging in deionized water, crushing a crude product, washing with boiled deionized water and absolute ethyl alcohol for 3 times respectively, and drying to obtain a powdery PK-1/PEI binary blend;
mixing 84g of PEEK powder and 16g of PK-1/PEI binary blend powder, adding the mixture into a high-speed stirrer, uniformly mixing the mixture at a high speed for 10min, putting the mixture into a vacuum oven to dry the mixture for 8 hours at 100 ℃, adding the dried mixture into a double-screw extruder, extruding the mixture at the temperature of 385 ℃ and the screw rotating speed of 40r/min, granulating, and drying the mixture for 12 hours at 120 ℃ in vacuum to obtain PEEK/PEI/PK-1 ternary alloy granules;
performing injection molding on the PEEK/PEI/PK-1 ternary alloy granules at 390 ℃ and 800bar, and annealing at 205 ℃ for 4 hours to obtain the PEEK/PEI/PK-1 ternary alloy.
Example 4
mixing 10g of PK-2 powder, 10g of PEI powder, 2g of LiCl and 150ml of LNMP, dissolving under stirring, discharging in deionized water, crushing a crude product, washing with boiled deionized water and absolute ethyl alcohol for 3 times respectively, and drying to obtain a powdery PK-2/PEI binary blend;
mixing 90g of PEEK powder and 10g of PK-2/PEI binary blend powder, adding the mixture into a high-speed stirrer, uniformly mixing the mixture at a high speed for 10min, putting the mixture into a vacuum oven to dry the mixture for 8 hours at 100 ℃, adding the dried mixture into a double-screw extruder, extruding the mixture at the temperature of 380 ℃ and the screw rotating speed of 40r/min, granulating, and drying the mixture for 12 hours at the temperature of 120 ℃ in vacuum to obtain PEEK/PEI/PK-2 ternary alloy granules;
And (3) carrying out injection molding on the PEEK/PEI/PK-2 ternary alloy granules at 400 ℃ and 880bar, and then annealing for 4.5 hours at 205 ℃ to obtain the PEEK/PEI/PK-1 ternary alloy.
Comparative example 1
Mixing 95g of PEEK powder and 5g of PEI powder, adding the mixture into a high-speed mixer, stirring the mixture at a high speed for 10min, uniformly mixing the mixture, putting the mixture into a vacuum oven to dry the mixture for 8 hours at the temperature of 100 ℃, adding the dried mixture into a double-screw extruder, extruding and granulating the mixture at the temperature of 380 ℃ and the screw rotating speed of 40r/min, and drying the mixture for 12 hours at the temperature of 120 ℃ in vacuum to obtain PEEK/PEI binary alloy granules;
Performing injection molding on the PEEK/PEI binary alloy granules at 390 ℃ and 800bar, and then annealing for 4 hours at 205 ℃ to obtain the PEEK/PEI binary alloy.
Example 5
The ternary alloys obtained in examples 1 to 4, the PEEEK/PEI binary alloy obtained in comparative example 1 and pure PEEK were respectively made into dumbbell-type tensile sample strips (length 75 mm/width 5 mm/thickness 2mm), bending sample strips (length 80 mm/width 10 mm/thickness 4mm) and friction sample strips by using a JIANDA-70 injection molding machine (Shenzhen Jianda mechanical Co., Ltd.). The coefficient of friction and the wear rate were measured according to GB-T3960-1983 using a UMT-2 multifunctional Friction tester (Bruker, Germany) and the results are shown in Table 1:
table 1: friction coefficient and wear rate of ternary alloy materials described in examples 1 to 4, binary alloy material described in comparative example 1, and pure PEEK resin
As can be seen from Table 1, the friction coefficient and the wear rate of the binary alloy PEEK/PEI in the comparative example 1 are larger than those of pure PEEK components, and the wear rate is slightly reduced, which indicates that the friction performance of the PEEK is not improved by adding PEI, while the friction coefficient and the wear rate of the ternary alloy materials in the examples 1 to 4 are lower than those of pure PEEK resins, which indicates that the friction performance of the PEEK can be improved by introducing aromatic polyamide, and the friction coefficients of the ternary alloy materials in the examples 1 to 4 are reduced by 4.7%, 11.6%, 16.3% and 9.3% respectively compared with the pure PEEK resins; the wear rates were reduced by 35.3%, 59.5%, 68.9% and 48.5%, respectively.
According to the GB/T1040-2006 and GB/T9341-2008 standards, a ShimadzuAG-1 type electronic universal tester is adopted to test the mechanical properties of the ternary alloy obtained in the examples 1-4, the PEEK/PEI binary alloy obtained in the comparative example 1 and a pure PEEK tensile bending sample strip, and the test results are shown in Table 2:
Table 2: mechanical properties of the ternary alloy materials described in examples 1 to 4, the binary alloy material described in comparative example 1, and pure PEEK resin
as can be seen from table 2, each mechanical property of the PEEK/PEI binary alloy in comparative example 1 is slightly reduced compared with that of the PEEK pure resin, which indicates that the addition of PEI is unfavorable for the mechanical property of PEEK, while the overall mechanical properties of the ternary alloy materials in examples 1 to 4 are similar to those of the PEEK pure resin, and even the tensile strength, bending strength and bending modulus are stronger than those of the PEEK pure resin, which indicates that the addition of aromatic polyamide improves the mechanical property of PEEK.
the foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. the ternary alloy containing the aromatic polyamide is prepared from the following raw materials in parts by weight:
70-94 parts of polyether-ether-ketone
3-20 parts of polyetherimide
3-10 parts of aromatic polyamide;
The aromatic polyamide is aromatic polyamide containing an ether ketone structure or aromatic polyamide containing naphthalene.
2. The ternary alloy containing aromatic polyamide according to claim 1, wherein said polyetheretherketone has a reduced viscosity of 0.8 to 1.0dL/g and a glass transition temperature of 142 to 144 ℃.
3. The aromatic polyamide-containing ternary alloy of claim 1, wherein the polyetherimide has a reduced viscosity of 0.4 to 0.6dL/g and a glass transition temperature of 215 to 217 ℃.
4. the aromatic polyamide-containing ternary alloy of claim 1, wherein the aromatic polyamide reduced viscosity is from 0.4 to 1.0 dL/g;
When the aromatic polyamide is aromatic polyamide containing an ether ketone structure, the glass transition temperature of the aromatic polyamide containing the ether ketone structure is 325-328 ℃;
When the aromatic polyamide is a naphthalene-containing aromatic polyamide, the glass transition temperature of the naphthalene-containing aromatic polyamide is 285-288 ℃.
5. The method for preparing the ternary alloy containing aromatic polyamide according to any one of claims 1 to 4, comprising the steps of:
Mixing aromatic polyamide, polyetherimide, cosolvent and organic solvent, and discharging in deionized water to obtain a binary blend of aromatic polyamide/polyetherimide;
And mixing the binary blend of the aromatic polyamide/polyetherimide with the polyether-ether-ketone, and sequentially performing extrusion, granulation, injection molding and annealing to obtain the ternary alloy containing the aromatic polyamide.
6. the preparation method of claim 5, wherein the cosolvent is one or more of calcium chloride, lithium chloride, magnesium chloride and methyl tri-n-butyl ammonium chloride;
The organic solvent is one or more of N, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and hexamethylphosphoramide.
7. The method of claim 5, wherein the extruding is performed in a twin screw extruder, the temperature of the extruding is 360 to 390 ℃, and the rotation speed of the twin screw extruder is 20 to 60 r/min.
8. The method according to claim 5, wherein the injection molding temperature is 380 to 400 ℃ and the injection molding pressure is 700 to 900 bar.
9. The method according to claim 5, wherein the annealing temperature is 200 to 210 ℃ and the annealing time is 3 to 5 hours.
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