CN111057373B - PPS wear-resistant material and preparation method thereof - Google Patents
PPS wear-resistant material and preparation method thereof Download PDFInfo
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- CN111057373B CN111057373B CN201911376291.3A CN201911376291A CN111057373B CN 111057373 B CN111057373 B CN 111057373B CN 201911376291 A CN201911376291 A CN 201911376291A CN 111057373 B CN111057373 B CN 111057373B
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F259/00—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention belongs to the technical field of wear-resistant materials, and particularly relates to a PPS wear-resistant material and a preparation method thereof. The PPS wear-resistant material is mainly prepared from polyphenylene sulfide resin, polytetrafluoroethylene and polytetrafluoroethylene grafted styrene, wherein the styrene content in the polytetrafluoroethylene grafted styrene is 20% -80%. The invention provides a wear-resistant material with good wear resistance and comprehensive mechanical properties: the compatibility of PPS and PTFE is effectively improved by adding the compatilizer PTFE-g-St, so that the mechanical strength and the wear resistance of the material are ensured. By adopting the preferred scheme of the invention, the wear-resisting life of the PPS wear-resisting material prepared by mixing the high-molecular-weight polytetrafluoroethylene and the low-molecular-weight polytetrafluoroethylene in proportion can be prolonged to more than 500 hours; the wear rate is only 0.0025 multiplied by 10‑6mm3V (N · m); meanwhile, the mechanical property of the wear-resistant material is not obviously reduced.
Description
Technical Field
The invention belongs to the technical field of wear-resistant materials, and particularly relates to a PPS wear-resistant material and a preparation method thereof.
Background
The material failure is mainly caused by 3 causes, i.e., corrosion, breakage and abrasion. For mechanical, electrical, and protective materials, wear is the primary cause of their failure. Tribological studies in many developed countries have found that material losses due to wear and accident losses are in the billions of dollars each year, while the special expenses for improving tribological conditions are also in the billions of dollars. Therefore, once one can improve or even avoid the occurrence of wear, a great economic effect will be produced. In recent years, serious abrasion loss caused by friction exists in the main national economic industries of metallurgy, processing, petroleum, transportation, aerospace, precision instruments and the like in China, and some advanced mechanical equipment or technologies cannot be applied due to the fact that the abrasion problem is not solved, so that the development of novel abrasion-resistant materials is not slow.
Polyphenylene Sulfide (PPS) is a novel special engineering plastic with excellent performance developed successfully by Phillips Petroleum in 1968. PPS has become the fastest-developing variety in engineering plastics in recent 10 years, and is known as novel plastic for the air injection era. PPS has excellent heat resistance, corrosion resistance, flame retardance, rigidity and electrical property, and also has excellent self-lubricating property and wear resistance (the friction coefficient is between 0.35 and 0.43), and the excellent heat conducting property (5 times that of common high polymers) enables the friction temperature rise to be lower, and the PPS has no corrosion effect on metals for several years. At present, PPS wear-resistant material is widely used for manufacturing bearings, gears, sealing rings and the like, and is a creditable preferred material due to self-lubricating property of the PPS wear-resistant material, especially in the occasions where lubricating oil cannot be used.
The research on the wear-resistant PPS material is mainly divided into the following aspects:
PPS/polymer composite
A. Polyphenylene sulfide/polytetrafluoroethylene (PPS/PTFE)
The advantages are that: if the molecular interaction force of PTFE is a positive interaction force, the molecular chain segments are easy to slip relatively, so that when the PTFE is subjected to the action of frictional shearing force, the PTFE can be peeled into flaky crystals, a layer of film is formed on the surface of the composite material, and the lubricating effect is achieved between the composite material and the opposite grinding surface. Therefore, the friction coefficient of the material can be greatly reduced by adding PTFE into the PPS matrix.
The disadvantages are that: the compatibility of PPS and PTFE is poor, and the comprehensive performance of the material can be influenced after the addition amount reaches a certain degree.
B. Polyphenylene sulfide/polyamide (PPS/PA)
The advantages are that: the PPS and the PA have good compatibility, and the industrial production is realized due to the mature process system.
The disadvantages are as follows: PA has no significant effect on reducing the coefficient of friction of PPS material.
PPS/inorganic filler composite
The advantages are that: the inorganic filler can reduce the adhesion between the transfer film and the surface of the high polymer, thereby reducing the friction coefficient and wear rate.
The disadvantages are as follows: due to the large addition of the inorganic filler, the mechanical properties of the material are significantly affected, and particularly the toughness is obviously reduced, so that the part is cracked.
PPS/nanoparticle composite
The advantages are that: the friction coefficient and the abrasion loss of the PPS can be obviously reduced by adding a small amount of nano particles, and the influence on the mechanical property of the material is small.
The disadvantages are as follows: the nano particles have small particle size, large specific surface area and large surface energy, so that agglomeration is easy to occur to influence the nano particles and the PPS.
Compatible composite materials of PPS/fiber matrix
The advantages are that: in the friction process, the fiber is used as a hard fulcrum to bear main pressure, so that the friction coefficient and the wear rate of the material are reduced.
The disadvantages are that: the breakage and falling of the fibers during the friction process can cause the loss of abrasion loss and form hard abrasive dust, thereby having negative influence on the friction performance of the material.
Relatively few reports are made at home and abroad on the modification of wear-resistant materials polyphenylene sulfide/polytetrafluoroethylene (PPS/PTFE). Through retrieval, Cao Wen Han et al adopt nanometer zirconium carbide modified filled polytetrafluoroethylene-polyphenylene sulfide composite material with friction and wear performance (polymer material science and engineering, 2018(34) 48-55.). The nano zirconium carbide can obviously improve the hardness and the wear resistance of the composite material, wherein the nano zirconium carbide/PTFE-PPS composite material with the volume fraction of 5 percent has the best friction and wear performance, and the wear rate is 5.8 multiplied by 10-6mm3And (N.m) is reduced by more than 130 times compared with the PTFE-PPS matrix. After the nano zirconia is added, although the wear resistance of the material is obviously improved, the inorganic filler particles are easy to agglomerate, so that the inorganic filler particles have poor dispersibility in a resin matrix and are easy to generate defects, thereby reducing the mechanical strength of the material. As can be seen from the mechanical property test data, the mechanical property corresponding to the optimal formula is only about 16MPa of tensile strength and only 11KJ/m of impact strength2Left and right. Therefore, the wear resistance and mechanical properties of the modified material still cannot meet the requirements of actual production. Therefore, there is also a need to provide a new PPS/PTFE modified material.
Disclosure of Invention
In order to solve the above problems in the prior art, it is an object of the present invention to provide a wear-resistant material with excellent wear resistance and comprehensive mechanical properties, which is improved based on PPS/PTFE.
Another object of the present invention is to provide a method for preparing the above wear-resistant material.
In order to achieve the above object, the present invention provides the following technical solutions:
the PPS wear-resistant material is mainly prepared from polyphenylene sulfide resin, polytetrafluoroethylene and polytetrafluoroethylene grafted styrene, wherein the styrene content of the polytetrafluoroethylene grafted styrene is 20% -80%.
The polytetrafluoroethylene grafted styrene PTFE-g-St is used as a compatilizer, improves the compatibility of PPS and PTFE so as to endow the material with good mechanical property, and in addition, the improvement of the compatibility of PPS and PTFE is also beneficial to improving the wear resistance of the material, and the combination of a surface PTFE molecular layer and a PPS matrix is tight and is not easy to fall off under the friction action.
According to the structural analysis of PTFE-g-St, the PTFE part in the PTFE-g-St is compatible with the PTFE component in the PPS/PTFE alloy because of the same substance, and the styrene (St) grafted in the PTFE-g-St is compatible with the PPS in the PPS/PTFE alloy because of similar molecular structures (both contain benzene rings), so that the compatibility of the PPS and the PTFE can be effectively improved after the PTFE-g-St is added, and the mechanical strength and the wear resistance of the material are ensured.
The test results also demonstrate this hypothesis. Through comparison, the grafted polymer prepared by respectively grafting polytetrafluoroethylene on maleic anhydride and glycidyl methacrylate is used for the wear-resistant material, and the wear-resistant material has better mechanical property but unsatisfactory wear resistance.
Preferably, the PPS wear-resistant material is mainly prepared from the following components in percentage by weight:
49.5-90% of polyphenylene sulfide resin, 5-50% of polytetrafluoroethylene and 0.5-10% of polytetrafluoroethylene grafted styrene, wherein the content range of styrene in the polytetrafluoroethylene grafted styrene is 20-80%.
Further preferably, the content of styrene in the polytetrafluoroethylene grafted styrene ranges from 60% to 70%. The polyphenylene sulfide material added with the corresponding compatilizer in the range has the best comprehensive performance of mechanical property and wear resistance.
Preferably, the polytetrafluoroethylene in the polytetrafluoroethylene-grafted styrene is low molecular weight PTFE, and the molecular weight range of the polytetrafluoroethylene is 1 ten thousand to 200 ten thousand, preferably 1 ten thousand to 50 ten thousand, and 1 ten thousand to 30 ten thousand.
As one embodiment, the wear-resistant material further comprises 0.5% -5% of N-butyl benzene sulfonamide. The N-butyl benzene sulfonamide is used as a micromolecule plasticizer, the movement capacity of PPS molecular chains can be improved, the dispersion effect of PTFE in a PPS matrix is improved, and in addition, the N-butyl benzene sulfonamide can migrate to the surface of a material due to low molecular weight to improve the self-lubricating property of the material and reduce abrasion.
Preferably, the wear-resistant material of the present invention may be added with other additives, such as a lubricant, according to requirements. However, not all the additives of conventional wear-resistant materials can be used in this patent, which would otherwise lead to a reduction in wear resistance or mechanical strength.
In the present invention, the polyphenylene sulfide resin PPS serves as a matrix portion, a continuous phase, and transmits an external action received by the material.
Preferably, the mass flow rate of the polyphenylene sulfide is in the range of 20g/10min to 300g/10 min.
Polyphenylene sulfides include linear and nonlinear.
The polytetrafluoroethylene PTFE is used as a solid lubricant, wherein low molecular weight PTFE is easy to migrate to the surface of a material due to strong molecular chain movement capacity of the PTFE, and can form a film to play a role in lubrication when the material is subjected to friction, but the polytetrafluoroethylene PTFE has the defects that the long-term wear resistance is poor, namely the wear resistance life is short, and the surface of a molded part is easy to peel to influence the appearance; the high molecular weight PTFE is fiberized under the action of screw shearing force in the mixing process to form a net structure, and plays a certain coating role on the low molecular weight PTFE, so that the wear resistance service life of the low molecular weight PTFE can be prolonged, the abrasion can be reduced, and the surface peeling phenomenon of a formed product can be improved.
Preferably, the content of the polyphenylene sulfide is 55-80%; more preferably 60 to 80% and 60 to 70%.
Preferably, the content of the polytetrafluoroethylene is 10% -40%; further preferably 15% -30% and 18% -30%.
The content of the polyphenylene sulfide and the content of the polytetrafluoroethylene are adjusted in the range according to the invention, and when the content of the polyphenylene sulfide exceeds (is higher than) the preferable range, the wear-resisting property of the wear-resisting material is obviously reduced; accordingly, when the content of polytetrafluoroethylene exceeds (exceeds) the preferred range, the mechanical properties of the wear-resistant material are significantly reduced.
As a preferred scheme of the invention, a mode of compounding two kinds of molecular weight PTFE is adopted to obtain good wear resistance and avoid possible defects.
Preferably, the polytetrafluoroethylene comprises high molecular weight Polytetrafluoroethylene (PTFE) and low molecular weight Polytetrafluoroethylene (PTFE), and the addition ratio of the low molecular weight PTFE to the high molecular weight PTFE is 1: 0.2-1: 5; wherein the molecular weight of the high molecular weight PTFE is 300-800 ten thousand, and the molecular weight of the low molecular weight PTFE is 1-200 ten thousand.
Further preferably, the ratio of the addition amount of the low molecular weight PTFE to the high molecular weight PTFE is 1: 0.5-1:5, 1: 0.8-1:5, 1: 0.2-1:2, 1: 0.5-1:2, 1: 0.5-1:3, 1: 0.5-1:4, 1: 1; for example, 1: 1.
Further preferably, the molecular weight of the high molecular weight PTFE is 300 ten thousand, 400 ten thousand, 500 ten thousand, 600 ten thousand, 700 ten thousand, 800 ten thousand, 550 ten thousand, 400-550 ten thousand.
Further preferably, the molecular weight of the low molecular weight PTFE ranges from 1 ten thousand to 150 ten thousand, from 1 ten thousand to 120 ten thousand, from 1 ten thousand to 110 ten thousand, from 1 ten thousand to 100 ten thousand, from 1 ten thousand to 90 ten thousand, from 1 ten thousand to 80 ten thousand, from 1 ten thousand to 70 ten thousand, from 1 ten thousand to 60 ten thousand, from 1 ten thousand to 50 ten thousand and from 1 to 30 ten thousand; for example, 1 ten thousand, 2 ten thousand, 5 ten thousand, 10 ten thousand, 20 ten thousand, 30 ten thousand, 50 ten thousand.
Different from the traditional PPS/PTFE wear-resistant material added with low-molecular-weight PTFE micro powder, the high-molecular-weight PTFE is introduced into the material, and the low-molecular-weight PTFE is wrapped by the low-molecular-weight PTFE by utilizing the characteristic that the low-molecular-weight PTFE is fiberized under the shearing action of a screw in the mixing process, so that the phenomenon that a film formed by the low-molecular-weight PTFE in the friction process is prematurely damaged due to low shearing strength is avoided, and the wear-resistant life is shortened.
The polytetrafluoroethylene grafted styrene is prepared by adopting an intermittent seeded emulsion copolymerization process, and comprises the following steps: adding PTFE dispersion liquid, the functional group monomer St to be grafted and an emulsifier into a reaction container, stirring and heating to 65-95 ℃, adding a polymerization accelerator, and continuing to react for 4-10h at constant temperature to obtain PTFE-g-St.
The post-treatment process after the reaction is as follows: filtering the precipitate to remove excessive impurities, drying the polymerization product, and pulverizing for use.
Preferably, the emulsifier is Sodium Dodecyl Sulfate (SDS) and/or polyoxyethylene octylphenol ether-10.
Preferably, the polymerization accelerator is potassium persulfate KPS.
Preferably, the PTFE to St mass ratio is between 0.1 and 3.
Preferably, SDS and OP-10 are used in an amount of 0.5 to 2% by mass of the St monomer; further preferably 0.8 to 1.5%; for example 1%.
Preferably, the amount of the potassium persulfate KPS is 0.3-1% of the mass of the St monomer; further preferably 0.3 to 0.6%; for example 0.4%.
The invention also provides a preparation method of the wear-resistant material, which comprises the following steps: weighing the materials according to the proportion, adding the materials into a high-speed mixer, uniformly mixing to obtain a premix, putting the premix into a double-screw extruder, melting, mixing and granulating, wherein the heating temperature is as follows: 250 ℃ and 350 ℃ and feeding frequency: 10-30Hz, screw rotation speed: 200 and 500 rpm.
The wear-resistant material prepared by the method is subjected to the following operations before performance detection: the extruded particles were dried at a temperature of 120-150 ℃ for 3-5h, after which test bars were molded on a horizontal injection molding machine.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention provides a wear-resistant material with good wear resistance and comprehensive mechanical properties: the compatibility of PPS and PTFE is effectively improved by adding the compatilizer PTFE-g-St, so that the mechanical strength and the wear resistance of the material are ensured.
(2) Long wear life: the invention takes the abrasion loss as 1000mg test materialThe abrasion loss of the material is found that the abrasion-resistant life of the alloy material prepared from the pure high molecular weight or low molecular weight polytetrafluoroethylene and the polyphenylene sulfide is not more than 200 h. But the preferred scheme of the invention is adopted, namely the wear-resisting life of the PPS wear-resisting material prepared by mixing the high-molecular-weight polytetrafluoroethylene and the low-molecular-weight polytetrafluoroethylene in proportion can be prolonged to more than 500 hours; the wear rate is only 0.0025 multiplied by 10-6mm3V (N · m); meanwhile, the mechanical property of the wear-resistant material is not obviously reduced.
Detailed Description
The method of the present invention is described below with reference to specific examples to make it easier to understand and grasp the technical solution of the present invention, but the present invention is not limited thereto. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified. Wherein the mass flow rate of the polyphenylene sulfide ranges from 20g/10min to 300g/10min, and comprises linearity and nonlinearity.
Examples 1 to 10
In each example, the composition ratios of the wear-resistant materials are shown in table 1 below. (weight%)
Table 1 each example provides the respective component distribution of the abrasion resistant material
The preparation method of the wear-resistant material comprises the following steps:
weighing the materials according to the proportion, adding the materials into a high-speed mixer, uniformly mixing to obtain a premix, putting the premix into a double-screw extruder, melting, mixing and granulating, wherein the heating temperature is as follows: 250-350 ℃ and feeding frequency: 10-30Hz, screw rotation speed: 200 and 500 rpm.
The wear-resistant material prepared by the method is subjected to the following operations before performance detection: the extruded particles were dried at 120-150 ℃ for 3-5h, after which test bars were molded on a horizontal injection molding machine.
The preparation method of the compatilizer polytetrafluoroethylene-grafted polytetrafluoroethylene comprises the following steps:
the polytetrafluoroethylene grafted styrene is prepared by adopting an intermittent seeded emulsion copolymerization process, and comprises the following steps: adding PTFE dispersion liquid, a functional group monomer St to be grafted and an emulsifier Sodium Dodecyl Sulfate (SDS) into a reaction container, stirring, heating to 65-95 ℃, adding a polymerization accelerator potassium persulfate (KPS), and continuously reacting for 4-10h at constant temperature to obtain PTFE-g-St.
The post-treatment process after the reaction is as follows: filtering the precipitate to remove excessive impurities, drying the polymerization product, and finally crushing for later use;
wherein the mass ratio of PTFE to St is 0.1-3;
Preferably, SDS and OP-10 are used in an amount of 1% by mass based on the mass of St monomer;
preferably, the amount of potassium persulfate KPS is 0.4% by mass of St monomer.
Performance test
1. Abrasion resistance test
The wear-resistant materials provided in the above examples were tested for wear resistance by a method according to the national standard GB/T3690 (300N load, 2m/s friction rate, 2h friction), and the results are shown in Table 2 below. Wherein, the service life refers to the wear-resisting time (unit is h) of a sample to be tested when the wear loss is 1000 mg; the wear rate is calculated in units of wear volume/(load × sliding distance): 10-6mm3/(N·m)。
Table 2 wear resistance of the wear resistant materials provided in the examples
2. Mechanical properties
The mechanical properties of the wear-resistant materials provided in the above examples were tested according to the national standard method, and the results are shown in table 3 below. Wherein, the tensile strength test standard is as follows: ISO 527(10mm/min test rate);
flexural strength test standard: ISO 178(2mm/min test rate);
the simple supported beam notch impact strength test standard is as follows: ISO 179 (type C notch).
Table 3 mechanical properties of the wear resistant materials provided in the examples
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. The PPS wear-resistant material is mainly prepared from the following components in percentage by weight;
49.5% -90% of polyphenylene sulfide resin, 5% -50% of polytetrafluoroethylene, 0.5% -10% of polytetrafluoroethylene grafted styrene and 0.5% -5% of N-butyl benzene sulfonamide, wherein the content range of styrene in the polytetrafluoroethylene grafted styrene is 20% -80%; the polytetrafluoroethylene comprises the following components in a mass ratio of 1: 1, wherein the molecular weight of the high molecular weight PTFE is 300-800 ten thousand, and the molecular weight of the low molecular weight PTFE is 1-200 ten thousand;
the sum of the weight percentages of the components is 100 percent.
2. The PPS wear resistant material according to claim 1, wherein the polytetrafluoroethylene grafted styrene has a styrene content ranging from 60% to 70%.
3. The PPS abrasion resistant material according to claim 1, wherein the polytetrafluoroethylene grafted styrene is low molecular weight PTFE having a molecular weight in the range of 1 ten thousand to 50 ten thousand.
4. The PPS abrasion resistant material according to claim 1, wherein the polytetrafluoroethylene grafted styrene is low molecular weight PTFE having a molecular weight in the range of 1 ten thousand to 30 ten thousand.
5. The PPS abrasion resistant material as defined in any one of claims 1-4, the preparation method of polytetrafluoroethylene grafted styrene, comprising the steps of: adding PTFE dispersion liquid, the functional group monomer St to be grafted and an emulsifier into a reaction container, stirring and heating to 65-95 ℃, adding a polymerization accelerator, and continuing to react for 4-10h at constant temperature to obtain PTFE-g-St.
6. The method of making the PPS wear resistant material of any of claims 1-4, including the steps of: weighing the components according to the proportion, adding the components into a high-speed mixer, uniformly mixing to obtain a premix, and putting the premix into a double-screw extruder for melting, mixing and granulating.
7. The method of claim 6, wherein the twin-screw extruder has the following operating parameters: heating temperature: 250-350 ℃ and feeding frequency: 10-30Hz, screw rotation speed: 200 and 500 rpm.
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| CN113444208A (en) * | 2021-09-02 | 2021-09-28 | 宁波能之光新材料科技股份有限公司 | Compatilizer of fluorinated ethylene propylene and preparation method and application thereof |
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