CN110684317A - Polyvinylidene fluoride reinforced polyether-ether-ketone alloy and preparation method thereof - Google Patents
Polyvinylidene fluoride reinforced polyether-ether-ketone alloy and preparation method thereof Download PDFInfo
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- CN110684317A CN110684317A CN201910947919.4A CN201910947919A CN110684317A CN 110684317 A CN110684317 A CN 110684317A CN 201910947919 A CN201910947919 A CN 201910947919A CN 110684317 A CN110684317 A CN 110684317A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/04—Polymer mixtures characterised by other features containing interpenetrating networks
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
Abstract
The invention relates to a polyvinylidene fluoride reinforced polyether-ether-ketone alloy which is characterized by comprising the following components in parts by weight: polyether ether ketone: 55-75 parts; polyvinylidene fluoride: 15-20 parts of a solvent; nylon 4T resin: 3-5 parts; high crystallinity polypropylene: 2-8 parts; first compatibilizer: 2-10 parts; a second compatibilizer: 1-2 parts; silane coupling agent: 0.1-1.5 parts; antioxidant: 0.1-0.5 part; a stabilizer: 0.1 to 0.5 portion. The invention has better compatibility, not only eliminates the salient points on the surface, but also enables the molecular chains of the polyether-ether-ketone, the nylon 4T and the high-crystallinity polypropylene to be crosslinked, and the molecular chains of the polyether-ether-ketone, the nylon 4T and the high-crystallinity polypropylene are mutually penetrated, thereby forming an interpenetrating network structure and enhancing the normal-temperature impact resistance of the product. Therefore, the wear resistance and impact resistance of the polyether-ether-ketone can be greatly improved without reducing the mechanical property of the polyether-ether-ketone, so that the polyether-ether-ketone can be applied to wider fields.
Description
Technical Field
The invention relates to a preparation method of a poly (ether-ketone) alloy, in particular to a polyvinylidene fluoride reinforced poly (ether-ketone) alloy and a preparation method thereof, belonging to the technical field of composite polymer materials and molding processing thereof.
Background
The polyether-ether-ketone (PEEK) resin is an engineering plastic with excellent performance, high temperature resistance, excellent mechanical performance, good self-lubricating property, chemical corrosion resistance and flame retardance. The method is widely applied to the scientific and technological fields of high-end machinery, nuclear engineering, aviation and the like. However, the impact resistance and wear resistance of the polyetheretherketone material are not particularly outstanding, so that the application of the polyetheretherketone material in more fields can be limited, the defects can be improved by reinforcing polyvinylidene fluoride (PVDF), and meanwhile, the appearance of the product can be seriously influenced by the surface bump problem caused by the addition of the PVDF.
Alloying is another important way to improve the defects of the polyetheretherketone material, and can realize the effect of 'making up for the deficiencies'. The key point of the alloying material for achieving the ideal effect is to realize good compatibility among different resins, and although the defects of polyether-ether-ketone are improved to a certain extent by the invention, the effects obtained by adopting the conventional compatibilizer system are limited. And the serious defect that salient points exist on the surface of the polyvinylidene fluoride reinforced polyether-ether-ketone material is difficult to improve, and the impact property of the polyvinylidene fluoride reinforced polyether-ether-ketone material at normal temperature is unstable.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a polyvinylidene fluoride reinforced polyether-ether-ketone alloy and a preparation method thereof aiming at the prior art, so that original performance advantages are ensured, surface salient points are eliminated, and stable impact performance at normal temperature is ensured.
The technical scheme adopted by the invention for solving the problems is as follows:
the polyvinylidene fluoride reinforced polyether-ether-ketone alloy is characterized by comprising the following components in parts by weight:
polyether ether ketone: 55 to 75 portions of
Polyvinylidene fluoride: 15-20 parts of
Nylon 4T resin: 3-5 parts of
High crystallinity polypropylene: 2-8 parts of
First compatibilizer: 2-10 parts of
A second compatibilizer: 1-2 parts of
Silane coupling agent: 0.1 to 1.5 portions
Antioxidant: 0.1 to 0.5 portion
A stabilizer: 0.1 to 0.5 portion
The first compatibilizer is prepared by melt grafting MA on PVDF by adopting a gamma ray pre-irradiation grafting method to prepare PVDF-g-MA;
wherein the second compatibilizer is dimethylacetamide.
Preferably, the polyether ether ketone has a melt index of 10-50 g/10min under the test conditions of a temperature of 230 ℃ and a pressure of 2.16 kg.
Preferably, the polyvinylidene fluoride has a melt index of 19-35 g/10min under the test conditions of a temperature of 230 ℃ and a pressure of 2.16 kg.
Preferably, the nylon 4T resin is a nylon 4T resin having a melt index greater than 58g/10min under test conditions of a temperature of 320 ℃ and a pressure of 2.16 kg.
Preferably, the high crystallinity polypropylene has a melt index greater than 20g/10min under test conditions of a temperature of 230 ℃ and a pressure of 2.16 kg.
Preferably, the silane coupling agent is an amino-functional silane, and the amino-functional silane coupling agent is KH-550, i.e., gamma-aminopropyltriethoxysilane.
Preferably, the antioxidant is one or a mixture of two of hindered phenol, hindered amine and phosphite antioxidant.
As a preference, the hindered phenol antioxidant may be tris [2, 4-di-t-butylphenyl ] phosphite, the hindered amine antioxidant is 3, 5-di-t-butyl-4-hydroxyphenylpropionyl-hexanediamine, and the phosphite antioxidant is pentaerythrityl tetrakis [ beta- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ].
Preferably, the stabilizer is zinc stearate.
A preparation method of polyvinylidene fluoride reinforced polyether-ether-ketone alloy comprises the following steps:
firstly, irradiating polyvinylidene fluoride powder by using Co-60 gamma rays with the radiation dose of 20kGy to enable polyvinylidene fluoride to generate free radicals, then uniformly mixing maleic anhydride with the mass fraction of 5% and the irradiated polyvinylidene fluoride, grafting in a double-helix mixing roll, finally cooling a graft by using water, and then drying and granulating to prepare a first compatibilizer;
step two, respectively weighing 55-75 parts of polyether-ether-ketone, 3-5 parts of nylon 4T resin, 2-8 parts of high-crystallinity polypropylene, 15-20 parts of polyvinylidene fluoride, 2-10 parts of first compatibilizer prepared in step one, 1-2 parts of second compatibilizer, 0.1-1.5 parts of silane coupling agent, 0.1-0.5 part of antioxidant and 0.1-0.5 part of stabilizer according to the formula dosage; then carrying out conventional drying treatment on the nylon 4T resin;
thirdly, putting the polyether-ether-ketone, the dried nylon 4T resin, the high-crystallinity polypropylene, the first compatibilizer, the second compatibilizer, the silane coupling agent, the antioxidant and the stabilizer into a high-speed mixer, and mixing at the rotating speed of 600-1200 rpm for 20-30min to obtain a premix;
step four, adding the premix obtained in the step three into a main feeding port of a double-screw extruder, placing polyvinylidene fluoride into a side feeding port of the double-screw extruder, performing melt blending, and then extruding and granulating to obtain a polyvinylidene fluoride reinforced polyether-ether-ketone alloy; wherein the screw rotating speed of the double-screw extruder is 500-600 r/min, and the melting temperature of the double-screw extruder is 340-380 ℃. .
Compared with the prior art, the invention has the advantages that:
the alloy system is prepared by selecting the polyether-ether-ketone and the polyvinylidene fluoride, the compatibility is better by adopting the special first compatibilizer and other components, the salient points on the surface are eliminated, the molecular chains of the polyether-ether-ketone, the nylon 4T and the high-crystallinity polypropylene are crosslinked, and the molecular chains of the polyether-ether-ketone, the nylon 4T and the high-crystallinity polypropylene are mutually penetrated, so that an interpenetrating network structure is formed, and the normal-temperature impact resistance of the product is enhanced. Therefore, the polyvinylidene fluoride reinforced polyether-ether-ketone alloy and the preparation method thereof can greatly improve the wear resistance and the impact resistance of the polyether-ether-ketone alloy without reducing the mechanical property of the polyether-ether-ketone alloy, so that the polyvinylidene fluoride reinforced polyether-ether-ketone alloy can be applied to wider fields.
Detailed Description
The present invention will be described in further detail with reference to examples.
A polyvinylidene fluoride reinforced polyether-ether-ketone alloy comprises the following components in parts by weight:
polyether ether ketone: 55 to 75 portions of
Polyvinylidene fluoride: 15-20 parts of
Nylon 4T resin: 3-5 parts of
High crystallinity polypropylene: 2-8 parts of
First compatibilizer: 2-10 parts of
A second compatibilizer: 1-2 parts of
Silane coupling agent: 0.1 to 1.5 portions
Antioxidant: 0.1 to 0.5 portion
A stabilizer: 0.1 to 0.5 portion
The first compatibilizer is prepared by melt grafting MA (maleic anhydride) on PVDF by adopting a gamma ray pre-irradiation grafting method to prepare PVDF-g-MA. The first compatibilizer greatly improves the compatibility of the poly (vinylidene fluoride) and the polyether-ether-ketone, and also greatly improves the compatibility of the polyether-ether-ketone, the nylon 4T and the high-crystallinity polypropylene.
The second compatibilizer is dimethylacetamide, and can form a new chemical bond between p-phenylene of polyether-ether-ketone, amide groups of nylon 4T and vinyl groups of high-crystallinity polypropylene, the new chemical bond can crosslink molecular chains of the polyether-ether-ketone, the nylon 4T and the high-crystallinity polypropylene, and the molecular chains of the polyether-ether-ketone, the nylon 4T and the high-crystallinity polypropylene penetrate through each other, so that an interpenetrating network structure is formed.
The polyether-ether-ketone has a melt index of 10-50 g/10min under the test conditions that the temperature is 230 ℃ and the pressure is 2.16 kg.
The polyvinylidene fluoride is polyvinylidene fluoride with a melt index of 19-35 g/10min under the test conditions that the temperature is 230 ℃ and the pressure is 2.16 kg.
Wherein the nylon 4T resin is a nylon 4T resin having a melt index greater than 58g/10min at a test condition of temperature 320 ℃ and pressure of 2.16 kg.
Wherein the high crystallinity polypropylene is a high crystallinity polypropylene having a melt index greater than 20g/10min at a test condition of a temperature of 230 ℃ and a pressure of 2.16 kg.
The silane coupling agent is amino functional group silane which is KH-550 (gamma-aminopropyltriethoxysilane), and the compatibility between polyvinylidene fluoride and polyether ether ketone can be effectively improved by using the amino functional group silane coupling agent.
Wherein the antioxidant is one or a mixture of two of hindered phenol, hindered amine and phosphite antioxidant. The hindered phenol antioxidant can be tris [2, 4-di-tert-butylphenyl ] phosphite, the hindered amine antioxidant can be 3, 5-di-tert-butyl-4-hydroxyphenylpropionyl-hexamethylenediamine, and the phosphite antioxidant can be tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propanoic acid ] pentaerythritol ester.
Wherein the stabilizer is zinc stearate.
The invention also discloses a preparation method of the polyvinylidene fluoride reinforced polyether-ether-ketone alloy, which comprises the following steps:
firstly, irradiating polyvinylidene fluoride powder by using Co-60 gamma rays with the radiation dose of 20kGy to enable polyvinylidene fluoride to generate free radicals, then uniformly mixing maleic anhydride with the mass fraction of 5% and the irradiated polyvinylidene fluoride, grafting in a double-helix mixing roll, finally cooling a graft by using water, and then drying and granulating to prepare a first compatibilizer;
step two, respectively weighing 55-75 parts of polyether-ether-ketone, 3-5 parts of nylon 4T resin, 2-8 parts of high-crystallinity polypropylene, 15-20 parts of polyvinylidene fluoride, 2-10 parts of first compatibilizer prepared in step one, 1-2 parts of second compatibilizer, 0.1-1.5 parts of silane coupling agent, 0.1-0.5 part of antioxidant and 0.1-0.5 part of stabilizer according to the formula dosage; then carrying out conventional drying treatment on the nylon 4T resin;
thirdly, putting the polyether-ether-ketone, the dried nylon 4T resin, the high-crystallinity polypropylene, the first compatibilizer, the second compatibilizer, the silane coupling agent, the antioxidant and the stabilizer into a high-speed mixer, and mixing at the rotating speed of 600-1200 rpm for 20-30min to obtain a premix;
step four, adding the premix obtained in the step three into a main feeding port of a double-screw extruder, placing polyvinylidene fluoride into a side feeding port of the double-screw extruder, performing melt blending, and then extruding and granulating to obtain a polyvinylidene fluoride reinforced polyether-ether-ketone alloy; wherein the screw rotating speed of the double-screw extruder is 500-600 r/min, and the melting temperature of the double-screw extruder is 340-380 ℃.
The raw material specifications used in the following specific examples 1 to 3 and comparative examples 1 to 2 are shown in Table 1.
Table 1: detailed description of the raw materials used in the specific examples and comparative examples
Firstly, preparing 10kg of irradiated polyvinylidene fluoride with free radicals by adopting a radiation grafting method, then uniformly mixing 500g of maleic anhydride and the irradiated polyvinylidene fluoride, grafting in a double-helix mixing roll, finally cooling a graft by using water, and then drying and granulating to prepare a first compatibilizer;
example 1
50.8KG of polyether-ether-ketone, 10KG of polyvinylidene fluoride, 5KG of dried nylon 4T resin, 5KG of high-crystallinity polypropylene, 0.5KG of silane coupling agent, 8KG of first compatibilizer, 4KG of second compatibilizer, 0.25KG of antioxidant 1010, 0.25KG of antioxidant 168 and 0.2KG of stabilizer zinc stearate are placed in a high-speed mixer to be stirred and mixed, the rotating speed of the high-speed mixer is 800rpm, and the mixing time is 25 min. And then, melting and mixing the mixed raw materials through a double-screw extruder, and extruding and granulating, wherein the screw rotating speed of the double-screw extruder is 500rpm, and the melting temperature of the extruder is set to be 340-380 ℃, so that the product 1 is finally obtained.
Example 2
Putting 53.8kg of polyether-ether-ketone, 5kg of polyvinylidene fluoride, 2.5kg of dried nylon 4T resin, 2.5kg of high-crystallinity polypropylene, 0.5kg of silane coupling agent, 10kg of first compatibilizer, 5kg of second compatibilizer, 0.25kg of antioxidant 1010, 0.25kg of antioxidant 168 and 0.2kg of stabilizer zinc stearate into a high-speed mixer, stirring and mixing, wherein the rotating speed of the high-speed mixer is 700rpm, and the mixing time is 30 min. And then, melting and mixing the mixed raw materials through a double-screw extruder, and extruding and granulating, wherein the screw rotating speed of the double-screw extruder is 550rpm, and the melting temperature of the extruder is set to be 340-380 ℃, so that the product 2 is finally obtained.
Example 3
43.8KG of polyether-ether-ketone, 10KG of polyvinylidene fluoride, 5KG of dried nylon 4T resin, 5KG of high-crystallinity polypropylene, 0.5KG of silane coupling agent, 10KG of first compatibilizer, 5KG of second compatibilizer, 0.25KG of antioxidant 1010, 0.25KG of antioxidant 168 and 0.2KG of stabilizer zinc stearate are placed in a high-speed mixer to be stirred and mixed, the rotating speed of the high-speed mixer is 1200rpm, and the mixing time is 30 min. And then, melting and mixing the mixed raw materials through a double-screw extruder, and extruding and granulating, wherein the screw rotating speed of the double-screw extruder is 600rpm, and the melting temperature of the extruder is set to be 340-380 ℃, so that the product 3 is finally obtained.
Comparative example 1
45kg of polyether-ether-ketone, 3.5kg of polyphenylene sulfide, 2.5kg of ultra-high molecular weight polyethylene, 0.5kg of sodium dodecyl sulfate, 8kg of PPS-G-MAH (polyphenylene sulfone grafted maleic anhydride), 0.25kg of antioxidant 1010 and 0.2kg of stabilizer barium stearate are placed in a high-speed mixer to be stirred and mixed, the rotating speed of the high-speed mixer is 750rpm, and the mixing time is 20 min. And then, melting and mixing the mixed raw materials through a double-screw extruder, and extruding and granulating, wherein the screw rotating speed of the double-screw extruder is 450rpm, and the melting temperature of the extruder is set to be 340-380 ℃, so that a product 4 is finally obtained.
Comparative example 2
43.8KG of polyether ether ketone, 3KG of polyphenylene sulfone resin, 2KG of polyphenylene oxide, 2.5KG of low-density polyethylene, 0.5KG of sodium dodecyl benzene sulfonate, 8KG of PPSU-G-MAH, 0.25KG of antioxidant 168 and 0.2KG of calcium stearate serving as a stabilizer are placed in a high-speed mixer to be stirred and mixed, the rotating speed of the high-speed mixer is 1100rpm, and the mixing time is 30 min. And then, melting and mixing the mixed raw materials through a double-screw extruder, and extruding and granulating, wherein the screw rotating speed of the double-screw extruder is 650rpm, and the melting temperature of the extruder is set to be 340-380 ℃, and finally obtaining the product 5.
Carrying out a correlation performance test on the products 1-5 prepared in the embodiments 1-3 and the comparative examples 1-2, and testing the mechanical properties of the products according to an ISO standard; the specific test results of the coefficient of friction of the test products according to the ISO8295 standard are shown in Table 2.
Table 2: and 1-5 performance test results of the product.
The above table shows that the polyvinylidene fluoride reinforced polyether-ether-ketone alloy prepared by the method disclosed by the invention integrates the excellent tensile property of polyether-ether-ketone, the good wear resistance and impact resistance of polyvinylidene fluoride, and shows excellent mechanical properties. By comparing the performance test results of the specific examples and the comparative examples, it can be found that the more the compatibilizer accounts for the total mass part in a certain range, the better and excellent performance of the reinforced alloy material is.
In addition to the above embodiments, the present invention also includes other embodiments, and any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of the claims of the present invention.
Claims (10)
1. The polyvinylidene fluoride reinforced polyether-ether-ketone alloy is characterized by comprising the following components in parts by weight:
polyether ether ketone: 55 to 75 portions of
Polyvinylidene fluoride: 15-20 parts of
Nylon 4T resin: 3-5 parts of
High crystallinity polypropylene: 2-8 parts of
First compatibilizer: 2-10 parts of
A second compatibilizer: 1-2 parts of
Silane coupling agent: 0.1 to 1.5 portions
Antioxidant: 0.1 to 0.5 portion
A stabilizer: 0.1 to 0.5 portion
The first compatibilizer is prepared by melt grafting MA on PVDF by adopting a gamma ray pre-irradiation grafting method to prepare PVDF-g-MA;
wherein the second compatibilizer is dimethylacetamide.
2. The polyvinylidene fluoride-reinforced polyetheretherketone alloy of claim 1, wherein the polyetheretherketone is a polyetheretherketone having a melt index of 10 to 50g/10min at a temperature of 230 ℃ and a pressure of 2.16 kg.
3. The polyvinylidene fluoride-reinforced polyether-ether-ketone alloy according to claim 1, wherein the polyvinylidene fluoride is polyvinylidene fluoride having a melt index of 19-35 g/10min under a test condition of a temperature of 230 ℃ and a pressure of 2.16 kg.
4. A polyvinylidene fluoride-reinforced polyetheretherketone alloy according to claim 1, wherein the nylon 4T resin is a nylon 4T resin having a melt index of greater than 58g/10min at a temperature of 320 ℃ and a pressure of 2.16kg under the test conditions.
5. A polyvinylidene fluoride-reinforced polyetheretherketone alloy according to claim 1, wherein the high crystallinity polypropylene is a high crystallinity polypropylene having a melt index of greater than 20g/10min at a test condition temperature of 230 ℃ and a pressure of 2.16 kg.
6. A polyvinylidene fluoride-reinforced polyetheretherketone alloy according to claim 1, wherein the silane coupling agent is an amino-functional silane which is KH-550 (gamma-aminopropyltriethoxysilane).
7. The polyvinylidene fluoride-reinforced polyetheretherketone alloy of claim 1, wherein the antioxidant is one or a mixture of two of hindered phenolic, hindered amine and phosphite antioxidants.
8. A polyvinylidene fluoride reinforced polyetheretherketone alloy according to claim 7, wherein the hindered phenolic antioxidant is tris [2, 4-di-tert-butylphenyl ] phosphite, the hindered amine antioxidant is 3, 5-di-tert-butyl-4-hydroxyphenylpropionyl-hexamethylenediamine, and the phosphite antioxidant is pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
9. A polyvinylidene fluoride-reinforced polyetheretherketone alloy according to claim 1, wherein the stabiliser is zinc stearate.
10. A preparation method of polyvinylidene fluoride reinforced polyether-ether-ketone alloy is characterized by comprising the following steps:
firstly, irradiating polyvinylidene fluoride powder by using Co-60 gamma rays with the radiation dose of 20kGy to enable polyvinylidene fluoride to generate free radicals, then uniformly mixing maleic anhydride with the mass fraction of 5% and the irradiated polyvinylidene fluoride, grafting in a double-helix mixing roll, finally cooling a graft by using water, and then drying and granulating to prepare a first compatibilizer;
step two, respectively weighing 55-75 parts of polyether-ether-ketone, 3-5 parts of nylon 4T resin, 2-8 parts of high-crystallinity polypropylene, 15-20 parts of polyvinylidene fluoride, 2-10 parts of first compatibilizer prepared in step one, 1-2 parts of second compatibilizer, 0.1-1.5 parts of silane coupling agent, 0.1-0.5 part of antioxidant and 0.1-0.5 part of stabilizer according to the formula dosage; then carrying out conventional drying treatment on the nylon 4T resin;
thirdly, putting the polyether-ether-ketone, the dried nylon 4T resin, the high-crystallinity polypropylene, the first compatibilizer, the second compatibilizer, the silane coupling agent, the antioxidant and the stabilizer into a high-speed mixer, and mixing at the rotating speed of 600-1200 rpm for 20-30min to obtain a premix;
step four, adding the premix obtained in the step three into a main feeding port of a double-screw extruder, placing polyvinylidene fluoride into a side feeding port of the double-screw extruder, performing melt blending, and then extruding and granulating to obtain a polyvinylidene fluoride reinforced polyether-ether-ketone alloy; wherein the screw rotating speed of the double-screw extruder is 500-600 r/min, and the melting temperature of the double-screw extruder is 340-380 ℃.
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Application publication date: 20200114 |