CN107353645B - Polyphenylene sulfide self-lubricating resin composition easy to crystallize and preparation method thereof - Google Patents
Polyphenylene sulfide self-lubricating resin composition easy to crystallize and preparation method thereof Download PDFInfo
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- 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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Abstract
The invention discloses a polyphenylene sulfide self-lubricating resin composition easy to crystallize and a preparation method thereof, wherein the composition comprises, by mass, 85-100 Parts of Polyphenylene Sulfide (PPS) and 1-15 parts of polytetrafluoroethylene. The preparation method comprises the following steps: PPS for engineering plastics with a melt flow rate of 150-800 g/10min and polytetrafluoroethylene powder with a melting point of 295-315 ℃ are premixed in a stirrer and then melted, mixed and granulated in a double-screw extruder to prepare the composite material. Compared with the existing PPS resin composition and composite material, the crystallization temperature can be raised by more than 10 ℃ when the PPS resin composition and the composite material are cooled from a melt, the PPS resin composition can be quickly crystallized during injection molding, and a room-temperature mold can also be used, so that the injection molding efficiency can be improved, and the processing energy consumption can be reduced. The mechanical strength of the product is equivalent to that of PPS resin, the friction coefficient can be reduced to below 60 percent of that of the PPS resin, and the wear rate can be reduced to 10 percent of that of the PPS resin.
Description
Technical Field
The invention belongs to the field of new materials, and particularly relates to a polyphenylene sulfide self-lubricating resin composition easy to crystallize and a preparation method thereof.
Background
Polyphenylene Sulfide (PPS) is an engineering plastic with excellent performance, becomes the sixth major variety of engineering plastics and the first major variety of special engineering plastics, is widely applied to the fields of electronics, electrics, automobiles, pharmaceutical chemicals, mechanical manufacturing and the like, and is mainly characterized by high temperature resistance, corrosion resistance, good dimensional stability, excellent mechanical strength and electrical performance. The disadvantages are that the impact resistance of the product is poor and the friction coefficient is high; in order to ensure the performance of the product, the temperature of the mold adopted during processing the product is higher (130-180 ℃). Among them, impact resistance can be improved by increasing molecular weight and reinforcing filling, and a friction coefficient can be partially improved by adding a low friction coefficient substance such as PTFE or the like, but the disadvantage of using a high temperature mold is difficult to be improved. The current concept of lowering the processing die temperature generally employs increasing the crystallization temperature (Tmc) of the PPS material as it cools from the melt and lowering the glass transition temperature (Tg).
US 5120804: Easily crystalline polyphenylene sulfonated polymer and preparation therof (Application No. 596661; application date: 1990-10-11; grant No. 5120804; grant date: 1992-06-09) and Japanese patent JP 2971930: 易結晶性ポリフェニレンスルフィド共重合体およぴその製造方法(Application No: JP 19900250138, filing date: 1990-09-21; filing date: JP2971930(B2), filing date: 1999-11-08) reports that in order to increase the crystallization rate of PPS, ethers or the like are added during the synthesis of PPS resin to perform copolymerization reaction, which can decrease the Tg of PPS to increase the crystallization rate at the processing temperature and improve the toughness of the final product, but this method lowers the use temperature of the product to some extent and also affects the corrosion resistance of the material. More commonly, an inorganic nucleating agent is added to commercial PPS to increase the crystallization rate of PPS, and although the addition of inorganic substances accelerates the crystallization of PPS within a certain range, the friction coefficient of the material cannot be reduced.
In order to reduce the friction coefficient of PPS, there are some research works ((1) Zhang Qing, Cheng, Wang gang, Lu ai, Wang Nu, PPS/PTFE composite material friction and wear performance research, Chinese plastics, 2007,21(11): 32-35; (2) polyphenyleneSulfide (per) fluoromonomer materials and processes for preparation and user of (application No.: US 2008067622008-08; Publication No.: S0040017, 2011-02-17); (3) Resin composition for polishing parts (application No.: DE4392144A, Publication Date: 07/02/1998; finish Date: 05/20/1993)); (4) wujianhua, flame sintering of plastics to form film, material protection, 1995, 28(10):21-22) selects perfluoropolymers such as PTFE, PFA, FEP and the like to be blended with PPS, generally, when the addition of the perfluoropolymers needs to be increased to more than 20%, the effect of reducing the friction coefficient is obvious, and at the moment, the toughness of the blended material is also improved, but the mechanical strength is obviously reduced.
Disclosure of Invention
In view of the above, the invention provides an easily crystallized polyphenylene sulfide self-lubricating resin composition and a preparation method thereof, aiming at the defects of long time consumption and high energy consumption in the processing process and the problem of higher material friction coefficient.
In order to solve the technical problem, the invention discloses a polyphenylene sulfide self-lubricating resin composition easy to crystallize, which comprises, by mass, 85-100 parts of polyphenylene sulfide and 1-15 parts of polytetrafluoroethylene.
Further, the polyphenylene sulfide is used as engineering plastics, and the melt flow rate of the polyphenylene sulfide is 150-800 g/10 min.
Furthermore, the melting point of the polytetrafluoroethylene is 295-315 ℃.
The invention also discloses a preparation method of the polyphenylene sulfide self-lubricating resin composition easy to crystallize, which comprises the following steps:
step 1, preparing polytetrafluoroethylene: putting commodity polytetrafluoroethylene powder into a polyethylene bag, putting the polyethylene bag into an electron accelerator for irradiation, kneading the polytetrafluoroethylene in the bag at times by utilizing the rotation of a sample table to a non-irradiation area so as to enable the irradiation to be uniform, opening the polyethylene bag in a ventilation cabinet after the irradiation is finished, and taking out the polyethylene bag after 1-5 hours;
step 2, weighing: weighing the following components in parts by mass: 85-100 parts of polyphenylene sulfide and 1-15 parts of polytetrafluoroethylene;
and 3, stirring and premixing the weighed polyphenylene sulfide and polytetrafluoroethylene uniformly in a stirrer, then melting and mixing in a double-screw extruder, extruding into strips, cooling the extruded strips in a cooling tank, and shearing into granules to prepare the easily-crystallized polyphenylene sulfide self-lubricating resin composition.
Further, the polyphenylene sulfide is polyphenylene sulfide resin for engineering plastics, and the melt flow rate of the polyphenylene sulfide is 150-800 g/10 min.
Furthermore, the melting point of the polytetrafluoroethylene is 295-315 ℃.
Further, the stirring speed in the step 3 is 45-75 r/min, and the stirring time is 3-8 min.
Further, the melt mixing conditions in the step 3 are that the four-section temperature set values of the screw extruder from the feed inlet to the discharge outlet are as follows: 260-270, 270-280, 295-305 and 290-300 ℃; the melt mixing time is 2 to 5 minutes.
Compared with the prior art, the invention can obtain the following technical effects:
1) compared with the existing PPS resin composition and composite material, the crystallization temperature can be raised by more than 10 ℃ when the PPS resin composition and the composite material are cooled from a melt, and the PPS resin composition is suitable for inorganic filler filling reinforcement and fiber reinforcement to manufacture the PPS composite material.
2) The easily crystallized polyphenylene sulfide self-lubricating resin composition can be quickly crystallized during injection molding, a room-temperature mold can be used, the injection molding efficiency is improved, the processing energy consumption is reduced, the friction coefficient of a product can be reduced to be below 60% of PPS resin, the wear rate can be reduced to be 10% of PPS, and the consistency of the quality of subsequent products is ensured.
Of course, it is not necessary for any one product in which the invention is practiced to achieve all of the above-described technical effects simultaneously.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is an SEM image of a brittle section of a composition of example 3 of the present invention and a distribution diagram of the elements thereof; wherein a is a brittle fracture surface, b is Carbon K alpha 1, c is Sulfur K alpha 1, and d is Fluorine K alpha 1;
FIG. 2 is an SEM image of a brittle fracture surface of a comparative example 1 composition of the present invention and an elemental distribution diagram thereof; wherein a is a brittle fracture surface, b is Carbon K alpha 1, c is Sulfur K alpha 1, and d is Fluorine K alpha 1.
Detailed Description
The following embodiments are described in detail with reference to the accompanying drawings, so that how to implement the technical features of the present invention to solve the technical problems and achieve the technical effects can be fully understood and implemented.
The invention discloses a polyphenylene sulfide self-lubricating resin composition easy to crystallize, which comprises, by mass, 85-100 Parts of Polyphenylene Sulfide (PPS) and 1-15 parts of Polytetrafluoroethylene (PTFE).
The PPS resin is used as engineering plastic (the melt flow rate is 150-800 g/10min, and the test is carried out at 316 ℃ and under the load of 5 kg); the melting point of the PTFE resin is 295-315 ℃ (DSC method test, 10 ℃/min heating rate, nitrogen atmosphere).
After the raw materials are mixed, the two raw materials are melted and uniformly mixed at the processing temperature and under the shearing, so that the technical problem that the conventional PTFE is not melted and is only dispersed in PPS under the processing condition is solved. Thus the present invention overcomes the disadvantage of a sharp interface between the two components; the addition amount of PTFE can be reduced, and the mechanical property of the PPS material is ensured. During cooling of the processed melt, the PTFE first crystallizes or is locally ordered, and this crystallized or locally ordered domain acts as a crystallization nucleating agent that significantly accelerates the crystallization of PPS, which results in higher temperatures at which PPS crystallizes from the melt, exhibiting easy crystallization characteristics.
The amount of PTFE added to PPS is not as large as possible, and is preferably within a certain range. This is because the strength and hardness of PTFE are significantly lower than those of PPS resins, and when the amount of PTFE added exceeds 15%, the mechanical strength and hardness of the blended material are significantly reduced; when the addition amount of PTFE is less than 1%, the influence on the PPS crystallization rate is small, and the improvement effect on the friction coefficient and the wear rate of the final blended material is not obvious, so that the blended material is better composed of 85-100 parts of PPS and 1-15 parts of PTFE.
The invention also discloses a preparation method of the polyphenylene sulfide self-lubricating resin composition easy to crystallize, which comprises the following steps:
step 1, preparing polytetrafluoroethylene: putting commercial PTFE powder into a polyethylene bag, putting the polyethylene bag into an electron accelerator for irradiation, kneading PTFE in the bag at intervals by utilizing the rotation of a sample table to a non-irradiation area so as to enable the irradiation to be uniform, opening the polyethylene bag in a fume hood after the irradiation is finished, and taking out the polyethylene bag after 1-5 hours;
step 2, weighing: weighing the following components in parts by mass: 85-100 parts of polyphenylene sulfide and 1-15 parts of polytetrafluoroethylene;
step 3, putting the weighed polyphenylene sulfide and polytetrafluoroethylene into a stirrer, stirring and mixing at the rotating speed of 45-75 revolutions per minute for 3-8 minutes at normal temperature, then basically mixing the raw materials uniformly, then melting and mixing in a double-screw extruder and extruding into strips, cooling the extruded strips in a cooling tank by tap water, and shearing into granules to prepare the easily crystallized polyphenylene sulfide self-lubricating resin composition; wherein, the melt mixing conditions are that the four-section temperature set values of the double-screw extruder from the feed inlet to the discharge outlet are as follows: 260-270, 270-280, 295-305 and 290-300 ℃; the melt mixing time is 2 to 5 minutes.
The prepared polyphenylene sulfide self-lubricating resin composition easy to crystallize has a crystallization temperature (Tmc) of more than 245 ℃ when the composition is cooled from a melt according to DSC analysis.
After the composition is dried at 120 ℃ for 4 hours, a test sample (room temperature mold) prepared by injection molding at 300 ℃ has the mechanical strength equivalent to that of PPS resin, the friction coefficient can be reduced to be less than 60 percent of that of the PPS resin, and the wear rate can be reduced to be 10 percent of that of the PPS.
When the composition is used for injection molding, the PTFE content is lower, and the PTFE has melt fluidity, so that the processing process is more convenient, the melt expansion phenomenon is basically eliminated, and the dimensional stability of an injection molded product is better.
Example 1
Premixing 20kg of PPS resin powder with the melt flow rate of 295g/10min and 2kg of PTFE powder with the melting point of 315 ℃, then carrying out melt mixing and extrusion granulation in a double-screw extruder, wherein the Tmc of the obtained composition is approximate to a single peak, and the peak temperature is 248 ℃; wherein the premixing condition is as follows: the rotating speed is 60 revolutions per minute, and the time is 5 minutes; the melt mixing conditions are that the four-section temperature set values of the double-screw extruder from the feed inlet to the discharge outlet are as follows: 260-270, 270-280, 295-305 and 290-300 ℃; the melt mixing time was 3 minutes.
Example 2
Premixing 20kg of PPS resin powder with the melt flow rate of 295g/10min and 2kg of PTFE powder with the melting point of 306 ℃, then carrying out melt mixing and extrusion granulation in a double-screw extruder, wherein the Tmc of the obtained composition is a single peak, and the peak temperature is 250 ℃; the melt mixing conditions are that the four-section temperature set values of the double-screw extruder from the feed inlet to the discharge outlet are as follows: 260-270, 270-280, 295-305 and 290-300 ℃; the melt mixing time was 3 minutes.
Example 3
Premixing 20kg of PPS resin powder with the melt flow rate of 295g/10min and 2kg of PTFE powder with the melting point of 295 ℃, then carrying out melt mixing and extrusion granulation in a double-screw extruder, wherein the Tmc of the obtained composition is a single peak, and the peak temperature is 250 ℃; the melt mixing conditions are that the four-section temperature set values of the double-screw extruder from the feed inlet to the discharge outlet are as follows: 260-270, 270-280, 295-305 and 290-300 ℃; the melt mixing time was 3 minutes.
Example 4
Premixing 20kg of PPS resin powder with the melt flow rate of 295g/10min and 0.2kg of PTFE powder with the melting point of 295 ℃, then carrying out melt mixing and extrusion granulation in a double-screw extruder, wherein the Tmc of the obtained composition is a single peak, and the peak temperature is 250 ℃; the melt mixing conditions are that the four-section temperature set values of the double-screw extruder from the feed inlet to the discharge outlet are as follows: 260-270, 270-280, 295-305 and 290-300 ℃; the melt mixing time was 3 minutes.
Example 5
Premixing 17kg of PPS resin powder with the melt flow rate of 150g/10min and 3kg of PTFE powder with the melting point of 315 ℃, then carrying out melt mixing and extrusion granulation in a double-screw extruder, wherein the Tmc of the obtained composition is approximate to a single peak, and the peak temperature is 249 ℃; wherein the premixing condition is as follows: the rotating speed is 45 revolutions per minute, and the time is 8 minutes; the melt mixing conditions are that the four-section temperature set values of the double-screw extruder from the feed inlet to the discharge outlet are as follows: 260-270, 270-280, 295-305 and 290-300 ℃; the melt mixing time was 2 minutes.
Example 6
Premixing 19.8kg of PPS resin powder with the melt flow rate of 800g/10min and 0.2kg of PTFE powder with the melting point of 295 ℃, and then carrying out melt mixing, extrusion and granulation in a double-screw extruder to obtain a composition, wherein the Tmc of the composition is a single peak, and the peak temperature is 250 ℃; wherein the premixing condition is as follows: the rotating speed is 75 revolutions per minute, and the time is 3 minutes; the melt mixing conditions are that the four-section temperature set values of the double-screw extruder from the feed inlet to the discharge outlet are as follows: 260-270, 270-280, 295-305 and 290-300 ℃; the melt mixing time was 5 minutes.
Example 7
Premixing 18kg of PPS resin powder with the melt flow rate of 500g/10min and 2kg of PTFE powder with the melting point of 305 ℃, then carrying out melt mixing and extrusion granulation in a double-screw extruder, wherein the Tmc of the obtained composition is a single peak, and the peak temperature is 250 ℃; wherein the premixing condition is as follows: the rotating speed is 55 revolutions per minute, and the time is 6 minutes; the melt mixing conditions are that the four-section temperature set values of the double-screw extruder from the feed inlet to the discharge outlet are as follows: 260-270, 270-280, 295-305 and 290-300 ℃; the melt mixing time was 4 minutes.
Comparative example 1
20kg of PPS resin powder having a melt flow rate of 295g/10min was premixed with 2kg of PTFE powder having a melting point of 329 ℃ and then melt-mixed in a twin-screw extruder and extrusion-granulated to obtain a composition having a Tmc of two peaks and peak temperatures of 239 ℃ and 314 ℃.
Comparative example 2
20kg of PPS resin having a melt flow rate of 295g/10min was subjected to melt extrusion pelletization in a twin-screw extruder to obtain pellets having a single peak Tmc and a peak temperature of 228 ℃.
The materials obtained in examples and comparative examples were injection-molded into standard test specimens, and the mechanical strength and frictional wear properties were measured, and the results are summarized in Table 1.
The performance test method comprises the following steps:
1. testing of Tmc
Taking 5-6 mg of sample, adding into N2Heating from 50 deg.C to 350 deg.C at a rate of 10 deg.C/min under atmosphere on DSC 204 type thermal analyzer of Netzsch, Germany, maintaining at 350 deg.C for 5min to eliminate thermal history, and cooling to 50 deg.C at the same rateDEG C; after stabilizing for 5min, the temperature is raised to 350 ℃ again at the same temperature raising rate, and a DSC curve of temperature raising-temperature lowering-secondary temperature raising is measured. Wherein Tmc is obtained from the temperature decreasing curve and the melting point is obtained from the second temperature increasing curve.
2. SEM-EDS test
The test sample bar formed by injection molding is brittle-broken in liquid nitrogen, and the fracture surface is placed on a stage stuck with conductive adhesive after the fracture surface is vacuum-sprayed with gold, and the surface appearance of the fracture surface of the sample is observed by using a JSM-5600LV (Japanese JEOL company) type scanning electron microscope. SEM-EDS the element distribution in the sample was observed, and the EDS mapping time was 300 seconds.
3. Tensile strength
The tensile strength of the samples was measured on an Instron model 5567 electronic tensile tester, according to GB/T1040.2-2006, at a tensile speed of 20 mm/min.
4. Impact strength
The samples were tested for impact strength at room temperature on an XJU-55 type cantilever beam impact tester according to GB/T1843-2008 standard.
5. Friction and wear
Friction and wear tests were carried out on an abrasion tester model M-200 according to the GB/T3960-1983 standard. The dual material used in the experiment is 45#The surface smoothness of the steel is ▽ 8(≈ 0.8 μm), the outer diameter d is approximatively 40mm, during the experiment, the sample is kept still, the friction pair (steel ring) performs sliding friction, the load is 200N, and the experimental environment temperature is 20 +/-5 ℃.
TABLE 1 results of Performance test of materials obtained in examples 1 to 7 and comparative examples 1 to 2
The results show that the mechanical strength and the abrasion resistance of all the samples of examples are superior to those of PPS (comparative example 2). The crystallization temperature Tmc of the blended material composed of the low-melting-point PTFE and the PPS is higher than that of the blended material prepared by the common PTFE and the PPS.
Taking two typical samples, namely, the sample of example 3 and the sample of comparative example 1 as examples, after the test bars are brittle, SEM and EDS images of brittle sections are shown in figures 1 and 2, which show that the low molecular weight PTFE in the material of the invention is dispersed more uniformly in the PPS resin matrix. This uniformity of dispersion is the main cause of the effect of the present invention.
While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. The polyphenylene sulfide self-lubricating resin composition easy to crystallize is characterized by comprising, by mass, 85-100 parts of polyphenylene sulfide and 1-15 parts of polytetrafluoroethylene;
the polyphenylene sulfide is used as engineering plastics, the melt flow rate of the polyphenylene sulfide is 150-800 g/10min, the melt flow rate is 316 ℃ under the test condition, and the load is 5 kg;
the melting point of the polytetrafluoroethylene is 295-315 ℃.
2. The preparation method of the polyphenylene sulfide self-lubricating resin composition easy to crystallize is characterized by comprising the following steps:
step 1, preparing polytetrafluoroethylene: putting commodity polytetrafluoroethylene powder into a polyethylene bag, putting the polyethylene bag into an electron accelerator for irradiation, kneading the polytetrafluoroethylene in the bag at times by utilizing the rotation of a sample table to a non-irradiation area so as to enable the irradiation to be uniform, opening the polyethylene bag in a ventilation cabinet after the irradiation is finished, and taking out the polyethylene bag after 1-5 hours;
step 2, weighing: weighing the following components in parts by mass: 85-100 parts of polyphenylene sulfide and 1-15 parts of polytetrafluoroethylene;
step 3, stirring and premixing the weighed polyphenylene sulfide and polytetrafluoroethylene uniformly in a stirrer, then melting and mixing in a double-screw extruder and extruding into strips, cooling the extruded strips in a cooling tank, and shearing into granules to prepare the easily crystallized polyphenylene sulfide self-lubricating resin composition;
the polyphenylene sulfide is polyphenylene sulfide resin for engineering plastics, the melt flow rate of the polyphenylene sulfide is 150-800 g/10min, the melt flow rate is 316 ℃ under the test condition, and the load is 5 kg;
the melting point of the polytetrafluoroethylene is 295-315 ℃.
3. The method according to claim 2, wherein the stirring speed in the step 3 is 45 to 75 rpm and the stirring time is 3 to 8 minutes.
4. The preparation method according to claim 2, wherein the melt mixing conditions in the step 3 are that the four-stage temperature setting value of the screw extruder from the feed port to the discharge port is: 260-270 ℃, 270-280 ℃, 295-305 ℃ and 290-300 ℃; the melt mixing time is 2 to 5 minutes.
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| CN101784611A (en) * | 2007-08-13 | 2010-07-21 | 德累斯顿协会莱布尼茨聚合物研究所 | Polyphenylene sulfide (per) fluoropolymer materials and its production and application |
| CN102216383A (en) * | 2008-09-26 | 2011-10-12 | 华福涂料公司 | Blended fluoropolymer coatings for rigid substrates |
| CN105860524A (en) * | 2016-04-29 | 2016-08-17 | 四川大学 | Thermoplastic low-friction wear-resistant composite material and preparation method thereof |
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| CN102216383A (en) * | 2008-09-26 | 2011-10-12 | 华福涂料公司 | Blended fluoropolymer coatings for rigid substrates |
| CN105860524A (en) * | 2016-04-29 | 2016-08-17 | 四川大学 | Thermoplastic low-friction wear-resistant composite material and preparation method thereof |
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