CN111944313A - Modified polyphenylene sulfide plastic composite material and preparation method thereof - Google Patents
Modified polyphenylene sulfide plastic composite material and preparation method thereof Download PDFInfo
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- CN111944313A CN111944313A CN202010830778.0A CN202010830778A CN111944313A CN 111944313 A CN111944313 A CN 111944313A CN 202010830778 A CN202010830778 A CN 202010830778A CN 111944313 A CN111944313 A CN 111944313A
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- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 110
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 110
- 239000002131 composite material Substances 0.000 title claims abstract description 78
- 239000004033 plastic Substances 0.000 title claims abstract description 33
- 229920003023 plastic Polymers 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000000047 product Substances 0.000 claims abstract description 47
- 238000001816 cooling Methods 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 40
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 37
- 239000003365 glass fiber Substances 0.000 claims abstract description 34
- 239000011787 zinc oxide Substances 0.000 claims abstract description 34
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 31
- 239000012764 mineral filler Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000011265 semifinished product Substances 0.000 claims abstract description 26
- 229920003048 styrene butadiene rubber Polymers 0.000 claims abstract description 26
- 239000000314 lubricant Substances 0.000 claims abstract description 25
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 24
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 24
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 24
- 239000007822 coupling agent Substances 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 18
- 238000001125 extrusion Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 47
- 238000002156 mixing Methods 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 36
- 238000005303 weighing Methods 0.000 claims description 10
- 239000010445 mica Substances 0.000 claims description 5
- 229910052618 mica group Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims 1
- 238000002844 melting Methods 0.000 abstract description 20
- 230000008018 melting Effects 0.000 abstract description 20
- 239000002245 particle Substances 0.000 description 19
- 238000005520 cutting process Methods 0.000 description 10
- 238000010008 shearing Methods 0.000 description 10
- 239000000654 additive Substances 0.000 description 8
- 230000000996 additive effect Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 229920001971 elastomer Polymers 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000806 elastomer Substances 0.000 description 4
- 238000001746 injection moulding Methods 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- RLKFNDFGXOQHQN-UHFFFAOYSA-N 2-nonylphenol;phosphorous acid Chemical compound OP(O)O.CCCCCCCCCC1=CC=CC=C1O.CCCCCCCCCC1=CC=CC=C1O.CCCCCCCCCC1=CC=CC=C1O RLKFNDFGXOQHQN-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 description 1
- 229940063655 aluminum stearate Drugs 0.000 description 1
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 1
- GWOWVOYJLHSRJJ-UHFFFAOYSA-L cadmium stearate Chemical compound [Cd+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O GWOWVOYJLHSRJJ-UHFFFAOYSA-L 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- UQLDLKMNUJERMK-UHFFFAOYSA-L di(octadecanoyloxy)lead Chemical compound [Pb+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O UQLDLKMNUJERMK-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 229920006258 high performance thermoplastic Polymers 0.000 description 1
- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000010128 melt processing Methods 0.000 description 1
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- QUTZUATVZPXUJR-UHFFFAOYSA-N trinonyl phosphite Chemical compound CCCCCCCCCOP(OCCCCCCCCC)OCCCCCCCCC QUTZUATVZPXUJR-UHFFFAOYSA-N 0.000 description 1
- QOQNJVLFFRMJTQ-UHFFFAOYSA-N trioctyl phosphite Chemical compound CCCCCCCCOP(OCCCCCCCC)OCCCCCCCC QOQNJVLFFRMJTQ-UHFFFAOYSA-N 0.000 description 1
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical group [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L81/02—Polythioethers; Polythioether-ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a modified polyphenylene sulfide plastic composite material and a preparation method thereof, wherein the modified polyphenylene sulfide plastic composite material comprises polyphenylene sulfide, glass fiber, nano styrene butadiene rubber, nano zinc oxide, inorganic mineral filler and master batch composite auxiliary agent; sequentially adding polyphenylene sulfide, nano styrene-butadiene rubber, nano zinc oxide and inorganic mineral filler in a high-speed stirrer to prepare a base material; adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer to prepare a master batch composite auxiliary agent; putting the master batch composite auxiliary agent and the base stock into a high-speed stirrer to prepare a primary product; placing the primary product into a double-screw extruder, and adding long glass fibers subjected to preheating and drying treatment in advance in the extrusion process to prepare a modified polyphenylene sulfide plastic composite semi-finished product; and putting the semi-finished product into a high-temperature and high-pressure die to be heated and melted, and then cooling and maintaining the pressure to obtain a finished product of the modified polyphenylene sulfide plastic composite material. The modified polyphenylene sulfide plastic provided by the invention has the advantages of low melting temperature, high toughness and strength, simple preparation method and low cost.
Description
Technical Field
The invention relates to a composite material and a preparation method thereof, in particular to a modified polyphenylene sulfide plastic composite material and a preparation method thereof.
Background
Polyphenylene Sulfide (PPS) is a high-performance thermoplastic resin with a main chain structure formed by alternately arranging benzene rings and sulfur atoms, has the advantages of high temperature resistance, radiation resistance, corrosion resistance, flame retardance, high modulus and the like, has wide application in the fields of electronics, electricity, automobile industry, mechanical industry, chemical industry and the like, and becomes the first large variety of special engineering plastics. However, pure PPS has low ductility, poor toughness, high melting point, which makes it easy to undergo thermooxidative crosslinking during melt processing molding, poor flowability, which makes molding difficult, and PPS is expensive compared to other plastics. Therefore, in order to lower the melting point of PPS, improve the strength and toughness of PPS, reduce the cost, and expand the range of personalized applications, it is necessary to modify PPS. The most common modification process is to incorporate a second component in PPS, for example to incorporate glass fibers for reinforcement or elastomers for toughening. The presence of the elastomer can cause the PPS matrix to generate brittle-tough transition, thereby achieving the toughening effect. However, elastomer dispersion and compatibility issues are key factors that limit PPS toughening. For example, Lee blends PPS with ethylene-glycidyl methacrylate copolymer (EGMA), and the toughness of the PPS/EGMA blend is maximized at 5% EGMA mass fraction. With continued increase in EGMA, the toughness of the PPS/EGMA blend decreases due to the poor compatibility of EGMA with PPS. At the same time, the increase in elastomer results in a decrease in the strength of the PPS base material. Thus, there is a conflicting opposition to the reinforcement and toughening of the prior methods. Therefore, achieving both reinforcement and toughening of PPS is a challenge in the art. In addition, the enhancement of PPS by adding rigid materials can cause the melting temperature of PPS composite materials to be increased, so that the PPS composite materials are limited in processing and application in some fields, such as difficult metal insert tin flowing caused by high melting temperature of PPS in the injection molding process of automobile functional injection molding parts. Meanwhile, the PPS automobile functional injection molding mainly works in an automobile engine compartment under the conditions of high temperature impact, high vibration strength and the like, so that the requirements on the strength and toughness of the PPS material are higher. Therefore, in order to widely use PPS in the field of automobile functional injection molding, the problem that the strength and toughness of PPS are increased while the melting temperature of PPS is reduced is urgently needed to be solved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a modified polyphenylene sulfide plastic composite material and a preparation method thereof, and the prepared material has low melting temperature, high toughness and high strength.
In order to achieve the purpose, the invention provides the following technical scheme: a modified polyphenylene sulfide plastic composite material comprises the following components in parts by weight: 40-60 parts of polyphenylene sulfide, 15-50 parts of glass fiber, 10-20 parts of nano styrene-butadiene rubber, 0.1-2 parts of nano zinc oxide, 5-10 parts of inorganic mineral filler and 10-20 parts of master batch composite auxiliary agent.
Further, the polyphenylene sulfide is linear polyphenylene sulfide.
Further, the nano zinc oxide is tetrapod-like zinc oxide whiskers.
Furthermore, the glass fiber is alkali-free long glass fiber with the diameter of 10-25 μm.
Further, the inorganic mineral filler is mica powder.
Furthermore, the master batch composite auxiliary agent is prepared by fusing polyphenylene sulfide with a phase solvent, an antioxidant, a lubricant and a coupling agent;
wherein: the phase solvent is one or two of polyolefin grafted maleic anhydride, PS compatilizer E-GMA-g-PS A4100, imide modified acrylic resin and epoxy resin modified polymer compatilizer, and the material has high polarity and reactivity by introducing strong polar reactive groups;
the antioxidant is one or a mixture of at least two of pentaerythritol tetra (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) and n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, phenyl phosphite, tris (nonylphenol) phosphite, tris (2, 4-di-tert-butylphenyl) phosphite, trinonyl phosphite and trioctyl phosphite;
the lubricant is metal soap lubricant, preferably one of zinc stearate, calcium stearate, lead stearate, barium stearate, magnesium stearate, cadmium stearate, aluminum stearate, sodium stearate and lithium stearate;
the coupling agent is a silane coupling agent, preferably one or a mixture of two of KH550, KH560, KH570, KH792, DL602 and DL 171.
A preparation method of a modified polyphenylene sulfide plastic composite material comprises the following steps:
the method comprises the following steps: weighing polyphenylene sulfide, glass fiber, nano styrene butadiene rubber, nano zinc oxide, inorganic mineral filler and master batch composite auxiliary agent according to the weight parts;
step two: sequentially adding polyphenylene sulfide, nano styrene-butadiene rubber, nano zinc oxide and inorganic mineral filler in a high-speed stirrer, stirring and heating to 150-200 ℃ to generate a base material;
step three: adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer, stirring and mixing uniformly, and heating to 150 ℃ and 200 ℃ to obtain a master batch composite auxiliary agent;
step four: putting the master batch composite auxiliary agent prepared in the third step into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 200 ℃ and 250 ℃, putting the base material prepared in the second step into the stirrer, stirring at a high speed at the temperature, and uniformly mixing to obtain a primary product;
step five: placing the primary product prepared in the fourth step into a double-screw extruder, and extruding when heating to 270-;
step six: adding long glass fibers subjected to preheating and drying treatment in advance in the extrusion process, cooling by cold water and granulating to obtain a modified polyphenylene sulfide plastic composite semi-finished product;
step seven: putting the semi-finished product prepared in the sixth step into a high-temperature high-pressure die, heating until the semi-finished product is completely molten, cooling to 260 ℃ at the speed of 50-100 ℃/min, and preserving heat for 5-10 min; and (3) rapidly pressurizing to 8-10MPa at the temperature, maintaining the pressure for 5-10min at the highest pressure, releasing the pressure, and naturally cooling to the normal temperature to obtain a finished product of the modified polyphenylene sulfide plastic composite material.
Compared with the prior art, the nano styrene-butadiene rubber, the nano zinc oxide and the inorganic mineral filler modifier with a proper structure are added into the polyphenylene sulfide at the same time, and the extrusion and temperature and pressure regulation processes are carried out, so that the modified polyphenylene sulfide plastic composite material provided by the invention has the advantages of low melting temperature, high toughness and strength, simple preparation method and low manufacturing cost.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
Detailed Description
The present invention is further described below.
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation steps of the invention are shown in figure 1.
The first embodiment is as follows:
sequentially weighing polyphenylene sulfide, glass fiber, nano styrene-butadiene rubber, nano zinc oxide, inorganic mineral filler, a phase solvent, an antioxidant, a lubricant and a coupling agent according to the weight fractions in the table 1, putting the polyphenylene sulfide, the nano styrene-butadiene rubber, the nano zinc oxide and the inorganic mineral filler into a high-speed stirrer, stirring and heating to 160 ℃, and mixing for 13 minutes to generate a base material; adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer according to the weight percentages in the table 1, heating the temperature to 160 ℃, uniformly mixing, and cooling to normal temperature to obtain a master batch composite additive; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 220 ℃, putting the base material, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding glass fiber in parts by weight at a feeding port of the 5 th section, and preparing a semi-finished product of material particles after extrusion, traction, cooling and particle cutting; the process conditions of the extruder are as follows: the temperature is 280 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute; putting the semi-finished product into a high-temperature high-pressure die, heating to be completely molten, cooling to 260 ℃ at the speed of 70 ℃/min, and keeping the temperature for 6 min; rapidly pressurizing to 9MPa at the temperature, and maintaining the pressure at the highest pressure for 6 min; releasing the pressure and naturally cooling to normal temperature to obtain a finished product of the modified polyphenylene sulfide plastic composite material; and (5) preparing the finished product into a standard sample strip, and carrying out various mechanical property tests and melting temperature tests. The test standards or methods and results are shown in table 2.
Example two:
sequentially weighing polyphenylene sulfide, glass fiber, nano styrene-butadiene rubber, nano zinc oxide, inorganic mineral filler, a phase solvent, an antioxidant, a lubricant and a coupling agent according to the weight fractions in the table 1, putting the polyphenylene sulfide, the nano styrene-butadiene rubber, the nano zinc oxide and the inorganic mineral filler into a high-speed stirrer, stirring and heating to 170 ℃, and mixing for 15 minutes to generate a base material; adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer according to the weight percentages in the table 1, heating the temperature to 170 ℃, uniformly mixing, and cooling to normal temperature to obtain a master batch composite additive; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 230 ℃, putting the base material, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding glass fiber in parts by weight at a feeding port of the 5 th section, and preparing a semi-finished product of material particles after extrusion, traction, cooling and particle cutting; the process conditions of the extruder are as follows: the temperature is 280 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute; putting the semi-finished product into a high-temperature high-pressure die, heating to be completely molten, cooling to 260 ℃ at the speed of 80 ℃/min, and keeping the temperature for 7 min; rapidly pressurizing to 9MPa at the temperature, and maintaining the pressure at the highest pressure for 7 min; releasing the pressure and naturally cooling to normal temperature to obtain a finished product of the modified polyphenylene sulfide plastic composite material; and (5) preparing the finished product into a standard sample strip, and carrying out various mechanical property tests and melting temperature tests. The test standards or methods and results are shown in table 2.
Example three:
sequentially weighing polyphenylene sulfide, glass fiber, nano styrene-butadiene rubber, nano zinc oxide, inorganic mineral filler, a phase solvent, an antioxidant, a lubricant and a coupling agent according to the weight fractions in the table 1, putting the polyphenylene sulfide, the nano styrene-butadiene rubber, the nano zinc oxide and the inorganic mineral filler into a high-speed stirrer, stirring and heating to 180 ℃, and mixing for 15 minutes to generate a base material; adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer according to the weight percentages in the table 1, heating the temperature to 180 ℃, uniformly mixing, and cooling to normal temperature to obtain a master batch composite additive; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 240 ℃, putting the base material, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding glass fiber in parts by weight at a feeding port of the 5 th section, and preparing a semi-finished product of material particles after extrusion, traction, cooling and particle cutting; the process conditions of the extruder are as follows: the temperature is 290 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute; putting the semi-finished product into a high-temperature high-pressure die, heating to be completely molten, cooling to 260 ℃ at a speed of 90 ℃/min, and keeping the temperature for 8 min; rapidly pressurizing to 9MPa at the temperature, and maintaining the pressure at the highest pressure for 8 min; releasing the pressure and naturally cooling to normal temperature to obtain a finished product of the modified polyphenylene sulfide plastic composite material; and (5) preparing the finished product into a standard sample strip, and carrying out various mechanical property tests and melting temperature tests. The test standards or methods and results are shown in table 2.
Example four:
sequentially weighing polyphenylene sulfide, glass fiber, nano styrene-butadiene rubber, nano zinc oxide, inorganic mineral filler, a phase solvent, an antioxidant, a lubricant and a coupling agent according to the weight fractions in the table 1, putting the polyphenylene sulfide, the nano styrene-butadiene rubber, the nano zinc oxide and the inorganic mineral filler into a high-speed stirrer, stirring and heating to 190 ℃, and mixing for 15 minutes to generate a base material; adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer according to the weight percentages in the table 1, heating the temperature to 190 ℃, uniformly mixing, and cooling to normal temperature to obtain a master batch composite additive; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 210 ℃, putting the base material, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding glass fiber in parts by weight at a feeding port of the 5 th section, and preparing a semi-finished product of material particles after extrusion, traction, cooling and particle cutting; the process conditions of the extruder are as follows: the temperature is 280 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute; putting the semi-finished product into a high-temperature high-pressure die, heating to be completely molten, cooling to 260 ℃ at the speed of 60 ℃/min, and keeping the temperature for 9 min; rapidly pressurizing to 9MPa at the temperature, and maintaining the pressure at the highest pressure for 9 min; releasing the pressure and naturally cooling to normal temperature to obtain a finished product of the modified polyphenylene sulfide plastic composite material; and (5) preparing the finished product into a standard sample strip, and carrying out various mechanical property tests and melting temperature tests. The test standards or methods and results are shown in table 2.
Example five:
sequentially weighing polyphenylene sulfide, glass fiber, nano styrene-butadiene rubber, nano zinc oxide, inorganic mineral filler, a phase solvent, an antioxidant, a lubricant and a coupling agent according to the weight fractions in the table 1, putting the polyphenylene sulfide, the nano styrene-butadiene rubber, the nano zinc oxide and the inorganic mineral filler into a high-speed stirrer, stirring and heating to 160 ℃, and mixing for 15 minutes to generate a base material; adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer according to the weight percentages in the table 1, heating the temperature to 160 ℃, uniformly mixing, and cooling to normal temperature to obtain a master batch composite additive; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 220 ℃, putting the base material, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding glass fiber in parts by weight at a feeding port of the 5 th section, and preparing a semi-finished product of material particles after extrusion, traction, cooling and particle cutting; the process conditions of the extruder are as follows: the temperature is 290 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute; putting the semi-finished product into a high-temperature high-pressure die, heating to be completely molten, cooling to 260 ℃ at the speed of 70 ℃/min, and keeping the temperature for 6 min; rapidly pressurizing to 9MPa at the temperature, and maintaining the pressure at the highest pressure for 6 min; releasing the pressure and naturally cooling to normal temperature to obtain a finished product of the modified polyphenylene sulfide plastic composite material; and (5) preparing the finished product into a standard sample strip, and carrying out various mechanical property tests and melting temperature tests. The test standards or methods and results are shown in table 2.
Example six:
sequentially weighing polyphenylene sulfide, glass fiber, nano styrene-butadiene rubber, nano zinc oxide, inorganic mineral filler, a phase solvent, an antioxidant, a lubricant and a coupling agent according to the weight fractions in the table 1, putting the polyphenylene sulfide, the nano styrene-butadiene rubber, the nano zinc oxide and the inorganic mineral filler into a high-speed stirrer, stirring and heating to 170 ℃, and mixing for 15 minutes to generate a base material; adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer according to the weight percentages in the table 1, heating the temperature to 170 ℃, uniformly mixing, and cooling to normal temperature to obtain a master batch composite additive; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 230 ℃, putting the base material, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding glass fiber in parts by weight at a feeding port of the 5 th section, and preparing a semi-finished product of material particles after extrusion, traction, cooling and particle cutting; the process conditions of the extruder are as follows: the temperature is 290 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute; putting the semi-finished product into a high-temperature high-pressure die, heating to be completely molten, cooling to 260 ℃ at the speed of 80 ℃/min, and keeping the temperature for 7 min; rapidly pressurizing to 9MPa at the temperature, and maintaining the pressure at the highest pressure for 7 min; releasing the pressure and naturally cooling to normal temperature to obtain a finished product of the modified polyphenylene sulfide plastic composite material; and (5) preparing the finished product into a standard sample strip, and carrying out various mechanical property tests and melting temperature tests. The test standards or methods and results are shown in table 2.
Example seven:
the following components in parts by weight were weighed in order: 40 parts of polyphenylene sulfide, 15 parts of glass fiber, 10 parts of nano styrene-butadiene rubber, 0.1 part of nano zinc oxide and 5 parts of inorganic mineral filler; putting polyphenylene sulfide, nano styrene-butadiene rubber, nano zinc oxide and inorganic mineral filler into a high-speed stirrer, stirring and heating to 150 ℃, and mixing for 15 minutes to generate a base material; and then weighing the master batch composite auxiliary agent: 8 parts of polyphenylene sulfide, 0.5 part of phase solvent, 0.5 part of antioxidant, 0.5 part of lubricant and 0.5 part of coupling agent, then adding master batch composite auxiliary ingredient in a high-speed stirrer, heating to 150 ℃, uniformly mixing, and cooling to normal temperature to obtain the master batch composite auxiliary; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 200 ℃, putting the base material, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding glass fiber in parts by weight at a feeding port of the 5 th section, and preparing a semi-finished product of material particles after extrusion, traction, cooling and particle cutting; the process conditions of the extruder are as follows: the temperature is 270 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute; putting the semi-finished product into a high-temperature high-pressure die, heating to be completely molten, cooling to 260 ℃ at the speed of 50 ℃/min, and keeping the temperature for 5 min; rapidly pressurizing to 8MPa at the temperature, and maintaining the pressure at the highest pressure for 5 min; releasing the pressure and naturally cooling to normal temperature to obtain the finished product of the modified polyphenylene sulfide plastic composite material.
Example eight:
the following components in parts by weight were weighed in order: 60 parts of polyphenylene sulfide, 50 parts of glass fiber, 20 parts of nano styrene butadiene rubber, 2 parts of nano zinc oxide and 10 parts of inorganic mineral filler; putting polyphenylene sulfide, nano styrene-butadiene rubber, nano zinc oxide and inorganic mineral filler into a high-speed stirrer, stirring and heating to 200 ℃, and mixing for 15 minutes to generate a base material; and then weighing the master batch composite auxiliary agent: 18 parts of polyphenylene sulfide, 0.5 part of phase solvent, 0.5 part of antioxidant, 0.5 part of lubricant and 0.5 part of coupling agent, then adding master batch composite auxiliary ingredient in a high-speed stirrer, heating to 200 ℃, uniformly mixing, and cooling to normal temperature to obtain the master batch composite auxiliary; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 250 ℃, putting the base material, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding glass fiber in parts by weight at a feeding port of the 5 th section, and preparing a semi-finished product of material particles after extrusion, traction, cooling and particle cutting; the process conditions of the extruder are as follows: the temperature is 300 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute; putting the semi-finished product into a high-temperature high-pressure die, heating to be completely molten, cooling to 260 ℃ at the speed of 100 ℃/min, and preserving heat for 10 min; rapidly pressurizing to 10MPa at the temperature, and maintaining the pressure at the highest pressure for 10 min; releasing the pressure and naturally cooling to normal temperature to obtain the finished product of the modified polyphenylene sulfide plastic composite material.
Comparative example one:
polyphenylene sulfide, glass fiber, a phase solvent, an antioxidant, a lubricant and a coupling agent are sequentially weighed according to the weight fractions in Table 1. Adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer according to the weight percentages in the table 1, heating the temperature to 180 ℃, uniformly mixing, and cooling to normal temperature to obtain a master batch composite additive; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 230 ℃, putting the polyphenylene sulfide, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding the glass fiber into the feeding port of the 5 th section according to the weight percentage, and preparing the finished product of the material particles after extrusion, traction, cooling and particle cutting. The process conditions of the extruder are as follows: the temperature is 290 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute; and (5) preparing the finished product into a standard sample strip, and carrying out various mechanical property tests and melting temperature tests. The test standards or methods and results are shown in table 2.
Comparative example two:
polyphenylene sulfide, glass fiber, a phase solvent, an antioxidant, a lubricant and a coupling agent are sequentially weighed according to the weight fractions in Table 1. Adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer according to the weight percentages in the table 1, heating the temperature to 170 ℃, uniformly mixing, and cooling to normal temperature to obtain a master batch composite additive; putting the master batch composite auxiliary agent into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 240 ℃, putting the polyphenylene sulfide, and uniformly stirring and mixing at a high speed to obtain a primary product; feeding the primary product into a double-screw extruder through a feeding device, and fully fusing through shearing, mixing and conveying; then adding the glass fiber into the feeding port of the 5 th section according to the weight percentage, and preparing a semi-finished product of material particles after extrusion, traction, cooling and grain cutting. The process conditions of the extruder are as follows: the temperature is 280 ℃, and the section is 1-10; screw rotation speed: 1200 revolutions per minute. And putting the semi-finished product into a high-temperature high-pressure die, heating to be completely molten, cooling to 260 ℃ at the speed of 80 ℃/min, and keeping the temperature for 6 min. At this temperature, the pressure was rapidly increased to 10MPa and maintained at the highest pressure for 6 min. Releasing the pressure and naturally cooling to normal temperature to obtain a finished product of the modified polyphenylene sulfide plastic composite material; and (5) preparing the finished product into a standard sample strip, and carrying out various mechanical property tests and melting temperature tests. The test standards or methods and results are shown in table 2.
As can be seen from Table 2, by comparing comparative example 1 with comparative example 2, the strength of the composite material can be remarkably increased by performing pressure control in the PPS melting and cooling process, and simultaneously, the toughness of the material is not reduced, and the crystallinity of the material is increased due to the high crystallization temperature, so that the strength is remarkably enhanced. The pressurization causes the movement and rearrangement of the crystalline units of the material, and the crystalline orientation is changed, so that the toughness of the material is not reduced.
By comparing example 1 and comparative example 2, or comparing example 4 and example 6, the strength of the composite material obtained by partially replacing glass fiber with low-price inorganic mineral filler mica powder is increased because the mica powder has a sheet-like structure and has a reinforcing effect by generating two-dimensional orientation during extrusion molding.
By comparing the examples 1, 2 and 3, the strength and toughness of the composite material are significantly improved by adding the nano zinc oxide, because the nano zinc oxide is the tetrapod-like zinc oxide whisker, and the tetrapod-like structure and the adjacent nano zinc oxide form a network structure, so that the force can be efficiently transmitted.
By comparing example 3 and example 4, the increase of the nano-rubber further reduces the melting temperature of the composite material, and the increase of the zinc oxide and the inorganic mineral filler further improves the toughness and the strength of the composite material.
By comparing the example 3 with the example 5, the mechanical property and the melting temperature of the composite material are basically unchanged after the low-price inorganic mineral filler mica powder partially replaces the polyphenylene sulfide, but the cost is reduced.
By comprehensively comparing examples 1-6 and comparative examples 1-2, the invention can simultaneously add nano styrene-butadiene rubber, nano zinc oxide and inorganic mineral filler modifier with proper structure into polyphenylene sulfide, and then obtain the modified polyphenylene sulfide composite material with low melting temperature, high toughness and strength through the extrusion process and the temperature and pressure regulation process. And because the cooperative regulation and control of the component proportion and the preparation method are simple, the modified polyphenylene sulfide composite material has lower manufacturing cost.
TABLE 1
TABLE 2
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any minor modifications, equivalent replacements and improvements made to the above embodiment according to the technical spirit of the present invention should be included in the protection scope of the technical solution of the present invention.
Claims (7)
1. The modified polyphenylene sulfide plastic composite material is characterized by comprising the following components in parts by weight: 40-60 parts of polyphenylene sulfide, 15-50 parts of glass fiber, 10-20 parts of nano styrene-butadiene rubber, 0.1-2 parts of nano zinc oxide, 5-10 parts of inorganic mineral filler and 10-20 parts of master batch composite auxiliary agent.
2. The modified polyphenylene sulfide plastic composite material as claimed in claim 1, wherein the polyphenylene sulfide is linear polyphenylene sulfide.
3. The modified polyphenylene sulfide plastic composite material as claimed in claim 1, wherein the nano zinc oxide is tetrapod-like zinc oxide whisker.
4. The modified polyphenylene sulfide plastic composite material as claimed in claim 1, wherein the glass fiber is alkali-free long glass fiber with a diameter of 10-25 μm.
5. The modified polyphenylene sulfide plastic composite material as claimed in claim 1, wherein the inorganic mineral filler is mica powder.
6. The modified polyphenylene sulfide plastic composite material as claimed in claim 1, wherein the master batch compounding aid is prepared by fusing polyphenylene sulfide with a phase solvent, an antioxidant, a lubricant and a coupling agent.
7. The method for preparing a modified polyphenylene sulfide plastic composite material as claimed in any one of claims 1 to 6, comprising the steps of:
the method comprises the following steps: weighing polyphenylene sulfide, glass fiber, nano styrene butadiene rubber, nano zinc oxide, inorganic mineral filler and master batch composite auxiliary agent according to the weight parts;
step two: sequentially adding polyphenylene sulfide, nano styrene-butadiene rubber, nano zinc oxide and inorganic mineral filler in a high-speed stirrer, stirring and heating to 150-200 ℃ to generate a base material;
step three: adding polyphenylene sulfide, a phase solvent, an antioxidant, a lubricant and a coupling agent into a high-speed stirrer, stirring and mixing uniformly, and heating to 150 ℃ and 200 ℃ to obtain a master batch composite auxiliary agent;
step four: putting the master batch composite auxiliary agent prepared in the third step into a high-speed stirrer, slowly stirring and heating, controlling the temperature at 200 ℃ and 250 ℃, putting the base material prepared in the second step into the stirrer, stirring at a high speed at the temperature, and uniformly mixing to obtain a primary product;
step five: placing the primary product prepared in the fourth step into a double-screw extruder, and extruding when heating to 270-;
step six: adding long glass fibers subjected to preheating and drying treatment in advance in the extrusion process, cooling by cold water and granulating to obtain a modified polyphenylene sulfide plastic composite semi-finished product;
step seven: putting the semi-finished product prepared in the sixth step into a high-temperature high-pressure die, heating until the semi-finished product is completely molten, cooling to 260 ℃ at the speed of 50-100 ℃/min, and preserving heat for 5-10 min; and (3) rapidly pressurizing to 8-10MPa at the temperature, maintaining the pressure for 5-10min at the highest pressure, releasing the pressure, and naturally cooling to the normal temperature to obtain a finished product of the modified polyphenylene sulfide plastic composite material.
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| CN114196205A (en) * | 2021-12-21 | 2022-03-18 | 江苏邦正新材料有限公司 | Preparation process for preparing high-purity pps nano material by using plasma |
| CN114634621A (en) * | 2021-12-21 | 2022-06-17 | 江苏邦正新材料有限公司 | Hydrothermal synthesis method of pps nano composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114196205A (en) * | 2021-12-21 | 2022-03-18 | 江苏邦正新材料有限公司 | Preparation process for preparing high-purity pps nano material by using plasma |
| CN114634621A (en) * | 2021-12-21 | 2022-06-17 | 江苏邦正新材料有限公司 | Hydrothermal synthesis method of pps nano composite material |
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