CN104744926A - High wear resistant and high self-lubrication continuous long fiber reinforced high temperature resistant nylon composite material and preparation method thereof - Google Patents
High wear resistant and high self-lubrication continuous long fiber reinforced high temperature resistant nylon composite material and preparation method thereof Download PDFInfo
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention belongs to the high temperature resistant nylon composite material field, and relates to a continuous long fiber reinforced high temperature resistant nylon composite material including the following components by weight: 100 parts of high temperature resistant nylon resin, 35-155 parts of continuous reinforced fiber, 1-15 parts of bismaleimide, 5-15 parts of a compatible agent A, 1-3 parts of a compatible agent B, 11-46 parts of a composite reinforced antiwear agent, 10-40 parts of a composite lubrication antifriction agent, 1.0-5.0 parts of a processing aid and 0.1-0.5 part of a curing agent. The high wear resistant and high self-lubrication continuous long fiber reinforced high temperature resistant nylon composite material has enough wear resistance, self lubrication property, mechanical properties, high temperature resistance and dimensional stability, and can be used in the manufacture of sliding parts such as gears, turbines, cam and other transmission parts and bearings, bushings, guide rails, pistons and other wear resistant, antifriction and self self-lubrication parts and general structural parts working in the high temperature environment.
Description
Technical field
The invention belongs to high temperature resistant nylon composite material field, relate to a kind of continuous long fiber and strengthen high temperature resistant nylon composite material and preparation method thereof.
Background technology
Engineering plastics generally have the features such as excellent self lubricity, wear resistance, low frictional properties and special seizure resistance, even if also can normally work when lubricating condition is bad, are desirable high-abrasive materials.Nylon structure regularity is good, crystallinity strong, and with other engineering plastics ratio, self lubricity is more outstanding, and wear loss and friction factor are all less, is more suitable for doing high-abrasive material.
In recent years, along with scientific-technical progress and industrial development, require more and more higher to properties of nylons, will as the abrasion-proof structure of high-strength light, normally can work under the very complicated exacting terms of operating mode such as high speed, high pressure and high temperature, but pure nylon resin cannot meet utilisation technology requirement, traditional method adopts glass fiber enhanced nylon, its mechanical property can be improved, but the self lubricity that extreme loss nylon itself is unique and wear resistance, so need the modification to carrying out self-lubricating and wear-resisting aspect while its enhancing modified, to meet product performance needs.
Semi-aromatic and all aromatic high temperature resistant nylon owing to having imported aromatic nucleus in main chain, and thermotolerance and mechanical property improve greatly, and water-intake rate declines, good stability of the dimension; Semi-aromatic and all aromatic high temperature resistant nylon have better wear resisting property in high temperature, high pressure, high vacuum with under having the occasion of chemical mediator, be especially suitable for use as slide unit as manufactured the driving parts such as gear, turbine, cam, and bearing, lining, guide rail, piston etc. are wear-resisting, anti-friction part and general structural parts.But independent semi-aromatic and semi-aromatic high temperature resistant nylon resin abrasion loss in high-speed friction is large, be difficult to meet the service requirements of the self-lubricating structural timber for a long time under high loads with surface abrasion resistance damage and low frictional properties matter.
Ultrahigh molecular weight polyethylene(UHMWPE) has the self-lubricating property of relatively low frictional coefficient excellence and excellent impelling strength and chemical stability, thus weaving is widely used in, papermaking, chemical industry, the fields such as mine and machinery, utilize the snappiness of ultrahigh molecular weight polyethylene(UHMWPE) excellence, self lubricity is improving shock resistance, the frictional coefficient of other performance as reduced high temperature resistant nylon that can also improve high temperature resistant nylon while reducing water-intake rate improves material wear ability etc., in order to improve wear resistance and the self lubricity of high temperature resistant nylon composite material further, adopt the method for adding ultrahigh molecular weight polyethylene(UHMWPE) and the composite lubricated low friction compound of tetrafluoroethylene.Ultrahigh molecular weight polyethylene(UHMWPE) intensity is not high on the other hand, rigidity is less, while its modified, high temperature resistant nylon, inevitably bring the reduction of intermingling material rigidity and intensity, in order to make material, there is excellent toughness, there is again high rigidity and intensity simultaneously, can be strengthened by inorganic nano-particle, whisker and fiber.
In existing fiber reinforced high-temperature-resistant nylon technology, one is glass fiber reinforcement high temperature resistant nylon, the processing condition also comparative maturity produced, but because glass fibre is poor in hydrolysis corrosive nature, cause the poor durability of galss fiber reinforced resin, especially, under the effect of long duration load, easily produce creep and its enhancement was lost efficacy, another kind is aramid fiber or fibre reinforced unsaturated polyester resin, and its physical and chemical performance is better, but price is too high, and cost performance is low, applies and is subject to certain restrictions, some physicals of basalt fibre fiber reinforced high-temperature-resistant nylon is greater than fiberglass reinforced unsaturated polyester resin, and basalt fibre hydrolysis, corrosion resistance nature is greater than glass fibre, relative to carbon fiber and aramid fiber, its cost performance is fairly obvious again, therefore the present invention utilizes short basalt fibre of cutting to strengthen high temperature resistant nylon, adopt the dipping coating equipment of continuous fiber reinforced thermoplastic material, compared with extruding fiber reinforced high-temperature-resistant nylon composite materials with conventional twin screw, in gained fiber reinforced high-temperature-resistant nylon composite materials particle, long fibre is arranged in parallel with each other along composite material granular length direction, and length is identical with composite material granular length, matrix material has better mechanical property, thermotolerance and dimensional stability.
The advantage such as hollow glass micropearl has that density is little, modulus is high, high temperature resistant and heat conductivity factor is little, is the new type functional inorganic filling material being usually used in filling modification of polymer materials in recent years, day by day attracts much attention.Hollow glass micropearl filled high polymer material not only can be increased wear-resisting, the resistance to compression of material and the performance such as fire-retardant, and its special spherical surface also can improve the processing fluidity of material.In addition, its surface gloss is good, can increase the surface luster of goods, reduces the dirt absorption on surface.Hollow glass micropearl wide material sources, cheap as the sustainable use important in inhibiting of a kind of novel environment-friendly materials to material.
Potassium titanate crystal whisker is good especially for the reinforced effects strengthening polymkeric substance, can be used for lightweight, the high specific strength of developing various novel high-level.Wear-resisting enhancing polymer composites, and be applicable to making different shape complexity, thin-walled, showing bright and clean beautiful accurate reinforcing member.
Patent CN1270189A provides a kind of preparation method with high self lubricity and high abrasion resistance nylon resin, although used polyvinyl resin with super-high molecular weight to be used as self-lubricating and anti-wear agent, but do not use high temperature resistant nylon in its patent, also use continuous lod; Patent CN101134844A provides a kind of flame-proof abrasion-resistant semi-fragrant polyamide composition, although used heat resistant polyamide in its patent, does not strengthen with continuous fiber, and anti-wear agent used is also different with self-lubricating agent; Patent CN1607219A provides a kind of high self-lubricating, wear-resisting, Reinforced Nylon engineering plastic alloy and manufacture method, although its patent has also used glass microballon, potassium titanate crystal whisker, tetrafluoroethylene and ultrahigh molecular weight polyethylene(UHMWPE), but it is not used continuous fibre and strengthens, also for adopting the dipping coating equipment of continuous fiber reinforced thermoplastic material to prepare matrix material.
Summary of the invention
Object of the present invention strengthens high temperature resistant nylon composite material and preparation method thereof providing one to have high-wearing feature and high self lubricity continuous long fiber.
The technical issues that need to address of the present invention have three: (1) provides a kind of nylon composite materials with excellent heat resistance; (2) the dipping coating equipment of continuous fiber reinforced thermoplastic material is adopted to obtain the high temperature resistant nylon composite material of excellent in mechanical performance; (3) the obtained high temperature resistant nylon composite material with high self lubricity and high-wearing feature.
In order to achieve the above object, the present invention adopts following technical scheme:
A kind of continuous long fiber strengthens high temperature resistant nylon composite material, is made up of the component comprising following weight part:
It is a kind of in semi-aromatic nylon between 290-330 DEG C or aromatic nylon or their composition that described high temperature resistant nylon resin is selected from fusing point; Wherein said semi-aromatic nylon is the Alkylenediamine polycondensation of terephthalic acid or m-phthalic acid and 4-12 carbon atom and obtains; Described aromatic nylon is terephthalic acid or a toluene dioctyl phthalate and Ursol D or mphenylenediamine polycondensation and obtains.
Described continuous fortifying fibre is one or more in continuous long glass fiber, continuous long basalt fibre, continuous long carbon fiber or continuous long aramid fiber, and Fibre diameter is 9-13 μm, preferred continuous long basalt fibre.
Described bismaleimides is diphenyl methane dimaleimide.
Described compatilizer A is one or more in high-density polycthylene grafted maleic anhydride or high-density polycthylene grafted glycidyl methacrylate.
Described compatilizer B is tetrabromo-bisphenol type epoxy resin.
Described composite strengthening anti-wear agent is made up of the potassium titanate crystal whisker of the hollow glass micropearl of 5-25 part, the nano silicon of 1-6 part and 5-15 part.
The particle diameter of described hollow glass micropearl is 10-24 μm, and tap density is 0.8-1.6g/cm
3.
The median size of described nano silicon is 30nm, and specific surface area is 600m
2/ g, loose density is 0.08g/cm
3, real density is 2.2g/cm
3.
Described potassium titanate crystal whisker diameter is 0.1-0.5 μm, length 3-15 μm.
Described composite lubricated low friction compound is made up of the tetrafluoroethylene of 5-15 part and the ultrahigh molecular weight polyethylene(UHMWPE) of 5-25 part, and wherein ultrahigh molecular weight polyethylene(UHMWPE) molecular weight is greater than 1,500,000.
Described processing aid is made up of the oxidation inhibitor of 0.5-1.5 part and the lubricant of 0.5-3.5 part.
Described oxidation inhibitor is β-(3; 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester (1076) of propionic acid, N; N'-is two-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (1098) or three [2.4-di-tert-butyl-phenyl] phosphorous acid ester (168) in one or more.
Described lubricant is one or more in ultra-high molecular weight polysiloxane or pentaerythritol stearate.
Described solidifying agent is one or more in mphenylenediamine, m-xylene diamine or quadrol.
Described continuous fiber strengthens fiber in high temperature resistant nylon composite material and is arranged in parallel with each other along composite material granular length direction, and length is identical with composite material granular length.
An above-mentioned preparation method with high-wearing feature and high self lubricity continuous fiber enhancing high temperature resistant nylon composite material, comprises the following steps:
(1) by high temperature resistant nylon resin, compatilizer A, composite strengthening anti-wear agent, composite lubricated low friction compound difference, drying;
(2) each component raw material of following weight part is taken according to said ratio: 100 parts of high temperature resistant nylon resins, 5-15 part compatilizer A, 1-15 part bismaleimides, 11-46 part composite strengthening anti-wear agent, the composite lubricated low friction compound of 10-40 part, 1.0-5.0 part processing aid and 0.1-0.5 part solidifying agent, join in high-speed mixer successively and mix, mixing time is 5-15 minute; By the material mixed, it is mixing to add twin screw extruder upstream addition mouth; Synchronously carry out the process of compatilizer B surface impregnation to 35-155 part continuous fiber, the compatilizer B be impregnated on continuous fibre is 1-3 part;
(3) continuous fiber synchronous for compatilizer B surface impregnation in (2) is added long fine coating machine die head, carry out infiltration coated, fibre content is adjusted to 35-155 part, continuous fortifying fibre surface impregnation 1-3 part compatilizer B by the engine speed of twin screw extruder and feeding frequency; Through cooling, traction, pelletizing, obtain continuous fiber and strengthen high temperature resistant nylon composite material.
In described step (1), high temperature resistant nylon raw material being placed in temperature is 110 DEG C of loft drier, dry 10h; Compatilizer A, composite strengthening anti-wear agent and composite lubricated low friction compound are placed in 80 DEG C of loft drier respectively, dry 4h.In described step (2), the engine speed of twin screw extruder is that 200-300 turns/min, and feeding frequency is 15-35Hz.The length being 4-6m/min control pellet by the pulling speed of adjustment dicing machine is 11-13mm, and the diameter being controlled pellet by the size 2.5mm of sizing mouth mould is 2.5mm;
In described step (2), the temperature of twin screw extruder is set as 275-335 DEG C.
The present invention has following beneficial effect:
(1) adopt nano silicon, hollow glass micropearl and the potassium titanate crystal whisker not only having had enhancement but also had wear-resisting effect to be used as composite strengthening anti-wear agent, make matrix material have wear-resisting while keep its mechanical property.
(2) adopt tetrafluoroethylene and ultrahigh molecular weight polyethylene(UHMWPE) to form composite lubricated low friction compound, make matrix material have excellent self lubricity and wear resistance.
(3) adopt functional compound grafted high density polyethylene to be used as the compatilizer of ultrahigh molecular weight polyethylene(UHMWPE) and high temperature resistant nylon, add the affinity of ultrahigh molecular weight polyethylene(UHMWPE) and high temperature resistant nylon two-phase.
(4) the dipping coating equipment of continuous fiber reinforced thermoplastic material is adopted, obtained tool height self lubricity and wear resistance and have in the high temperature resistant nylon composite material particle of high strength and thermotolerance, long fibre is arranged in parallel with each other along composite material granular length direction, and length is identical with composite material granular length, impart the better mechanical property of matrix material, thermotolerance and dimensional stability.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
The median size of the nano silicon described in following examples is 30nm, and specific surface area is 600m
2/ g, loose density is 0.08g/cm
3, real density is 2.2g/cm
3.
Embodiment 1
(1) poly-paraphenylene terephthalamide's decamethylene diamine being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted maleic anhydride, hollow glass micropearl, (particle diameter is 10 μm, and tap density is 1.6g/cm
3), silicon-dioxide, potassium titanate crystal whisker (diameter is 0.1 μm, and length is 15 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) be placed in 80 DEG C of loft drier respectively, dry 4h;
(2) by 100 parts of poly-paraphenylene terephthalamide's decamethylene diamines, 8 parts of diphenyl methane dimaleimides, 15 parts of high-density polycthylene grafted maleic anhydrides of compatilizer A, 36 parts of composite strengthening anti-wear agent (15 parts of hollow glass micropearls, 6 parts of nano silicons, 15 parts of potassium titanate crystal whiskers), 40 parts of composite lubricated low friction compound (15 parts of tetrafluoroethylene, 25 portions of ultrahigh molecular weight polyethylene(UHMWPE)s), 5 parts of processing aid (1.0 part of 1098 oxidation inhibitor, 0.5 part of 168 oxidation inhibitor, 3.5 parts of ultra-high molecular weight polysiloxane) and 0.5 part of mphenylenediamine join in high-speed mixer successively and mix, mixing time is 15 minutes, by the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing, tetrabromo-bisphenol type epoxy resin surface dip treating is synchronously carried out to 155 parts of continuous long basalt fibres that diameter is 9 μm, weigh continuous long basalt fibre before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 3 parts,
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long basalt fibre and add long fine coating machine die head, carry out infiltration coated, continuous long basalt fibre content is adjusted to 155 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 300 turns/min, feeding frequency is 15Hz, be 5m/min by adjusting the pulling speed of dicing machine, the length controlling pellet is 12mm, the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm, through cooling, traction, pelletizing, obtain that there is high-wearing feature and the poly-paraphenylene terephthalamide's decamethylene diamine matrix material of the continuous long basalt fibre enhancing of high self lubricity.
Embodiment 2
(1) poly-hexamethylene terephthalamide-co-hexamethylene adipamide multipolymer being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted maleic anhydride, hollow glass micropearl, (particle diameter is 10 μm, tap density is 1.6g/cm3), (diameter is 0.1 μm for silicon-dioxide, potassium titanate crystal whisker, length is 15 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) divide in 80 DEG C of loft drier, dry 4h;
(2) by 100 parts of poly-hexamethylene terephthalamide-co-hexamethylene adipamide multipolymers, 8 parts of diphenyl methane dimaleimides, 15 parts of high-density polycthylene grafted maleic anhydrides, 36 parts of composite strengthening anti-wear agent (15 parts of hollow glass micropearls, 6 parts of nano silicons, 15 parts of potassium titanate crystal whiskers), 40 parts of composite lubricated low friction compound (15 parts of tetrafluoroethylene, 25 portions of ultrahigh molecular weight polyethylene(UHMWPE)s), 5 parts of processing aid (1.0 part of 1076 oxidation inhibitor, 0.5 part of 168 oxidation inhibitor, 3.5 parts of ultra-high molecular weight polysiloxane) and 0.5 part of mphenylenediamine join in high-speed mixer successively and mix, mixing time is 15 minutes, by the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing, tetrabromo-bisphenol type epoxy resin surface dip treating is synchronously carried out to 155 parts of continuous long basalt fibres that diameter is 9 μm, weigh continuous long basalt fibre before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 3 parts,
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous fiber and add long fine coating machine die head, carry out infiltration coated, continuous long basalt fibre content is adjusted to 155 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 300 turns/min, feeding frequency is 15Hz, be 5m/min by adjusting the pulling speed of dicing machine, the length controlling pellet is 12mm, the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm, through cooling, traction, pelletizing, obtain that there is high-wearing feature and the poly-hexamethylene terephthalamide-co-hexamethylene adipamide copolymer composite of the continuous long basalt fibre enhancing of high self lubricity.
Embodiment 3
(1) poly-paraphenylene terephthalamide's nonamethylene diamine being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted maleic anhydride, hollow glass micropearl, (particle diameter is 10 μm, tap density is 1.6g/cm3), (diameter is 0.1 μm for silicon-dioxide, potassium titanate crystal whisker, length is 15 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) be placed in 80 DEG C of loft drier respectively, dry 4h;
(2) by 100 parts of poly-paraphenylene terephthalamide's nonamethylene diamines, 8 parts of diphenyl methane dimaleimides, 15 parts of high-density polycthylene grafted maleic anhydrides, 36 parts of composite strengthening anti-wear agent (15 parts of hollow glass micropearls, 6 parts of nano silicons, 15 parts of potassium titanate crystal whiskers), 40 parts of composite lubricated low friction compound (15 parts of tetrafluoroethylene, 25 portions of ultrahigh molecular weight polyethylene(UHMWPE)s), 1.5 parts of processing aid (1.0 part of 1098 oxidation inhibitor, 0.5 part of 168 oxidation inhibitor, 3.5 parts of ultra-high molecular weight polysiloxane) and 0.5 part of mphenylenediamine join in high-speed mixer successively and mix, mixing time is 15 minutes, by the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing, tetrabromo-bisphenol type epoxy resin surface dip treating is synchronously carried out to 155 parts of continuous long basalt fibres that diameter is 9 μm, weigh continuous long basalt fibre before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 3 parts,
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long basalt fibre and add long fine coating machine die head, carry out infiltration coated, continuous long basalt fibre content is adjusted to 155 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 300 turns/min, feeding frequency is 15Hz, be 5m/min by adjusting the pulling speed of dicing machine, the length controlling pellet is 12mm, the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm, through cooling, traction, pelletizing, obtain that there is high-wearing feature and the poly-paraphenylene terephthalamide's nonamethylene diamine matrix material of the continuous long basalt fibre enhancing of high self lubricity.
Embodiment 4
(1) polyphthalamide being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted maleic anhydride, hollow glass micropearl, (particle diameter is 10 μm, tap density is 1.6g/cm3), (diameter is 0.1 μm for silicon-dioxide, potassium titanate crystal whisker, length is 15 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) be placed in 80 DEG C of loft drier respectively, dry 4h;
(2) by 100 parts of polyphthalamides, 8 parts of diphenyl methane dimaleimides, 15 parts of high-density polycthylene grafted maleic anhydrides, 36 parts of composite strengthening anti-wear agent (15 parts of hollow glass micropearls, 6 parts of nano silicons, 15 parts of potassium titanate crystal whiskers), 40 parts of composite lubricated low friction compound (15 parts of tetrafluoroethylene, 25 portions of ultrahigh molecular weight polyethylene(UHMWPE)s), 5 parts of processing aid (0.5 part of 1098 oxidation inhibitor, 0.5 part of 1076 oxidation inhibitor, 0.5 part of 168 oxidation inhibitor, 3.5 parts of ultra-high molecular weight polysiloxane) and 0.5 part of mphenylenediamine join in high-speed mixer successively and mix, mixing time is 15 minutes, by the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing, tetrabromo-bisphenol type epoxy resin surface dip treating is synchronously carried out to 155 parts of continuous long basalt fibres that diameter is 9 μm, weigh continuous long basalt fibre before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 3 parts,
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long basalt fibre and add long fine coating machine die head, carry out infiltration coated, continuous long basalt fibre content is adjusted to 155 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 300 turns/min, and feeding frequency is 15Hz.Be 5m/min by adjusting the pulling speed of dicing machine; the length controlling pellet is 12mm; the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm; through cooling, traction, pelletizing, obtain that there is high-wearing feature and the continuous long basalt fibre enhancing polyphthalamide composite material of high self lubricity.
Embodiment 5
(1) poly-paraphenylene terephthalamide 12 carbon diamines being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted glycidyl methacrylate, hollow glass micropearl, (particle diameter is 17 μm, and tap density is 1.2g/cm
3), silicon-dioxide, potassium titanate crystal whisker (diameter is 0.3 μm, and length is 9 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) be placed in 80 DEG C of loft drier respectively, dry 4h;
(2) by 100 parts of poly-paraphenylene terephthalamide 12 carbon diamines, 15 parts of diphenyl methane dimaleimides, 10 parts of high-density polycthylene grafted glycidyl methacrylate, 38.5 parts of composite strengthening anti-wear agent (25 parts of hollow glass micropearls, 3.5 parts of nano silicons, 10 parts of potassium titanate crystal whiskers), 25 parts of composite lubricated low friction compound (10 parts of tetrafluoroethylene, 15 portions of ultrahigh molecular weight polyethylene(UHMWPE)s), 5 parts of processing aid (1.5 part of 1098 oxidation inhibitor, 3.5 parts of pentaerythritol stearates) and 0.3 part of quadrol join in high-speed mixer successively and mix, mixing time is 15 minutes, by the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing, synchronously carry out tetrabromo-bisphenol type epoxy resin surface dip treating to 95 parts of continuous long basalt fibres, weigh continuous long basalt fibre before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 2 parts,
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long basalt fibre and add long fine coating machine die head, carry out infiltration coated, continuous long basalt fibre content is adjusted to 95 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 300 turns/min, and feeding frequency is 25Hz.Be 6m/min by adjusting the pulling speed of dicing machine; the length controlling pellet is 11mm; the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm; through cooling, traction, pelletizing, obtain that there is high-wearing feature and the poly-paraphenylene terephthalamide 12 carbon diamines matrix material of the continuous long basalt fibre enhancing of high self lubricity.
Embodiment 6
(1) poly-phthalyl decamethylene diamine being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted glycidyl methacrylate, hollow glass micropearl, (particle diameter is 17 μm, and tap density is 1.2g/cm
3), silicon-dioxide, potassium titanate crystal whisker (diameter is 0.3 μm, and length is 9 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) be placed in 80 DEG C of loft drier respectively, dry 4h;
(2) 100 parts of poly-phthalyl decamethylene diamines, 10 parts of diphenyl methane dimaleimides, 5 parts of high-density polycthylene grafted glycidyl methacrylate, 11 parts of composite strengthening anti-wear agents (5 parts of hollow glass micropearls, 1 part of nano silicon, 5 parts of potassium titanate crystal whiskers), 20 parts of composite lubricated low friction compounds (15 portions of tetrafluoroethylene, 5 portions of ultrahigh molecular weight polyethylene(UHMWPE)s), 5 parts of processing aids (1.5 part of 1098 oxidation inhibitor, 3.5 parts of pentaerythritol stearates) and 0.1 part of mphenylenediamine are joined in high-speed mixer successively and mixed, mixing time is 5 minutes; By the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing; Synchronously carry out tetrabromo-bisphenol type epoxy resin surface dip treating to 35 parts of continuous long glass fibers that diameter is 11 μm, weigh continuous long glass fiber before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 1 part;
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long glass fiber and add long fine coating machine die head, carry out infiltration coated, continuous long glass fiber content is adjusted to 35 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 200 turns/min, feeding frequency is 35Hz, be 4m/min by adjusting the pulling speed of dicing machine, the length controlling pellet is 13mm, the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm, through cooling, traction, pelletizing, obtain that there is high-wearing feature and high self lubricity continuous long glass fiber enhancing polyphthalamide composite material.
Embodiment 7
(1) poly-phthalyl hexanediamine-co-hexamethylene adipamide multipolymer being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted maleic anhydride, hollow glass micropearl, (particle diameter is 17 μm, and tap density is 1.2g/cm
3), silicon-dioxide, potassium titanate crystal whisker (diameter is 0.3 μm, and length is 9 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) be placed in 80 DEG C of loft drier respectively, dry 4h;
(2) by 100 parts of poly-phthalyl hexanediamine-co-hexamethylene adipamide multipolymers, 10 parts of diphenyl methane dimaleimides, 10 parts of high-density polycthylene grafted maleic anhydrides, 28.5 parts of composite strengthening anti-wear agent (15 parts of hollow glass micropearls, 3.5 parts of nano silicons, 10 parts of potassium titanate crystal whiskers), 30 parts of composite lubricated low friction compound (15 parts of tetrafluoroethylene, 15 portions of ultrahigh molecular weight polyethylene(UHMWPE)s), 1 part of processing aid (0.5 part of 1098 oxidation inhibitor, 0.5 part of ultra-high molecular weight polysiloxane) and 0.3 part of mphenylenediamine join in high-speed mixer successively and mix, mixing time is 15 minutes, by the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing, synchronously carry out tetrabromo-bisphenol type epoxy resin surface dip treating to 95 parts of continuous long carbon fibers that diameter is 11 μm, weigh continuous long carbon fiber before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 2 parts,
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long carbon fiber and add long fine coating machine die head, carry out infiltration coated, continuous long carbon fiber content is adjusted to 95 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 250 turns/min, feeding frequency is 20Hz, be 6m/min by adjusting the pulling speed of dicing machine, the length controlling pellet is 11mm, the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm, through cooling, traction, pelletizing, obtain that there is high-wearing feature and high self lubricity continuous long carbon fiber enhancing polyphthalamide composite material.
Embodiment 8
(1) poly-phthalyl nonamethylene diamine being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted maleic anhydride, high-density polycthylene grafted glycidyl methacrylate, hollow glass micropearl, (particle diameter is 24 μm, and tap density is 0.8g/cm
3), silicon-dioxide, potassium titanate crystal whisker (diameter is 0.5 μm, and length is 3 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) be placed in 80 DEG C of loft drier respectively, dry 4h;
(2) by 100 parts of polyphthalamides, 8 parts of diphenyl methane dimaleimides, 5 parts of high-density polycthylene grafted maleic anhydrides, 5 parts of high-density polycthylene grafted glycidyl methacrylate, 28.5 parts of composite strengthening anti-wear agent (15 parts of hollow glass micropearls, 3.5 parts of nano silicons, 10 parts of potassium titanate crystal whiskers), 30 parts of composite lubricated low friction compound (5 parts of tetrafluoroethylene, 25 portions of ultrahigh molecular weight polyethylene(UHMWPE)s), 3 parts of processing aid (1.0 part of 1098 oxidation inhibitor, 2.0 parts of pentaerythritol stearates) and 0.3 part of quadrol join in high-speed mixer successively and mix, mixing time is 15 minutes, by the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing, synchronously carry out tetrabromo-bisphenol type epoxy resin surface dip treating to the continuous long aramid fiber that diameter 95 parts is 13 μm, weigh continuous long aramid fiber before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 2 parts,
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long aramid fiber and add long fine coating machine die head, carry out infiltration coated, continuous long aramid fiber content is adjusted to 95 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 300 turns/min, feeding frequency is 25Hz, be 4m/min by adjusting the pulling speed of dicing machine, the length controlling pellet is 13mm, the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm, through cooling, traction, pelletizing, obtain that there is high-wearing feature and the continuous long aramid fiber enhancing polyphthalamide composite material of high self lubricity.
Embodiment 9
(1) poly-paraphenylene terephthalamide's decamethylene diamine, polyphthalamide being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted maleic anhydride, high-density polycthylene grafted glycidyl methacrylate, hollow glass micropearl, (particle diameter is 10 μm, and tap density is 1.6g/cm
3), silicon-dioxide, potassium titanate crystal whisker (diameter is 0.1 μm, and length is 15 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) be placed in 80 DEG C of loft drier respectively, dry 4h;
(2) by 50 parts of poly-paraphenylene terephthalamide's decamethylene diamines, 50 polyphthalamide parts, 1 part of diphenyl methane dimaleimide, 5 parts of high-density polycthylene grafted maleic anhydrides, 5 parts of high-density polycthylene grafted glycidyl methacrylate, 46 parts of composite strengthening anti-wear agent (25 parts of hollow glass micropearls, 6 parts of nano silicons, 15 parts of potassium titanate crystal whiskers), 25 parts of composite lubricated low friction compound (15 parts of tetrafluoroethylene, 10 portions of ultrahigh molecular weight polyethylene(UHMWPE)s), 3.5 parts of processing aid (1.0 part of 1098 oxidation inhibitor, 0.5 part of 168 oxidation inhibitor, 1.0 parts of pentaerythritol stearates, 1.0 parts of ultra-high molecular weight polysiloxane), 0.25 part of m-xylene diamine and 0.25 part of quadrol join in high-speed mixer successively and mix, mixing time is 15 minutes, by the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing, synchronously carry out tetrabromo-bisphenol type epoxy resin surface dip treating to 155 parts of continuous long glass fibers that diameter is 11 μm, weigh continuous long glass fiber before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 3 parts,
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long glass fiber and add long fine coating machine die head, carry out infiltration coated, continuous long basalt fibre content is adjusted to 155 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 300 turns/min, feeding frequency is 15Hz, be 5m/min by adjusting the pulling speed of dicing machine, the length controlling pellet is 12mm, the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm, through cooling, traction, pelletizing, obtain that there is high-wearing feature and high self lubricity continuous long glass fiber enhancing polyphthalamide composite material.
Comparative example 1
(1) poly-paraphenylene terephthalamide's decamethylene diamine being placed in temperature is 110 DEG C of loft drier, dry 10h;
(2) 100 parts of poly-paraphenylene terephthalamide's decamethylene diamines, 8 parts of diphenyl methane dimaleimides, 1.0 part of 1098 oxidation inhibitor, 0.5 part of 168 oxidation inhibitor, 3.5 parts of ultra-high molecular weight polysiloxane and 0.5 part of mphenylenediamine are joined in high-speed mixer successively and mixed, mixing time is 15 minutes; By the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing; Synchronously carry out tetrabromo-bisphenol type epoxy resin surface dip treating to the continuous long basalt fibre that diameter is 9 μm, weigh continuous long basalt fibre before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 3 parts;
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long basalt fibre and add long fine coating machine die head, carry out infiltration coated, continuous long basalt fibre content is adjusted to 79 parts by the engine speed of twin screw extruder and feeding frequency, wherein the engine speed of twin screw extruder is 280 turns/min, feeding frequency is 35Hz, be 5m/min by adjusting the pulling speed of dicing machine, the length controlling pellet is 12mm, the diameter being controlled pellet by the size (2.5mm) of sizing mouth mould is 2.5mm, through cooling, traction, pelletizing, obtain that there is high-wearing feature and the poly-paraphenylene terephthalamide's decamethylene diamine matrix material of the continuous long basalt fibre enhancing of high self lubricity.
Comparative example 2
(1) poly-paraphenylene terephthalamide's decamethylene diamine being placed in temperature is 110 DEG C of loft drier, dry 10h; By high-density polycthylene grafted maleic anhydride, hollow glass micropearl, (particle diameter is 10 μm, and tap density is 1.6g/cm
3), silicon-dioxide, potassium titanate crystal whisker (diameter is 0.1 μm, and length is 15 μm), tetrafluoroethylene and molecular weight be 2,500,000 ultrahigh molecular weight polyethylene(UHMWPE) be placed in 80 DEG C of loft drier respectively, dry 4h;
(2) 100 parts of poly-paraphenylene terephthalamide's decamethylene diamines, 8 parts of diphenyl methane dimaleimides, 15 parts of high-density polycthylene grafted maleic anhydrides, 15 parts of hollow glass micropearls, 6 parts of nano silicons, 15 parts of potassium titanate crystal whiskers, 15 parts of tetrafluoroethylene, 25 parts of ultrahigh molecular weight polyethylene(UHMWPE)s, 1.0 part of 1098 oxidation inhibitor, 0.5 part of 168 oxidation inhibitor, 3.5 parts of ultra-high molecular weight polysiloxane and 0.5 part of mphenylenediamine are joined in high-speed mixer successively and mixed, mixing time is 15 minutes; By the material mixed, add and be set as that the twin screw extruder upstream addition mouth of 275-335 DEG C is mixing; Synchronously carry out tetrabromo-bisphenol type epoxy resin surface dip treating to the continuous long basalt fibre that diameter is 9 μm, weigh continuous long basalt fibre before and after surface impregnation process, the add-on that both difference can calculate tetrabromo-bisphenol type epoxy resin is 3 parts;
(3) tetrabromo-bisphenol type epoxy resin surface in (2) is flooded synchronous continuous long basalt fibre and add introducing twin screw extruder downstream macrofiber charging opening, the amount controlling basalt fibre is 155 parts, wherein the engine speed of twin screw extruder is 300 turns/min, and feeding frequency is 15Hz; Through extruding check rod, namely granulation obtains matrix material.
The embodiment with high-wearing feature and high self lubricity continuous fiber enhancing high temperature resistant nylon composite material obtained by this invention and comparative example performance see the following form 1:
Table 1
Drawn the following conclusions by the test data of table 1: (1) can find out prepared continuous fiber reinforced composite materials mechanical property by upper table performance and heat-drawn wire is high, abrasion of rolling are little, and the properties of embodiment 1 is best, is most preferred embodiment; (2) composite strengthening anti-wear agent and composite lubricated low friction compound is not added in the matrix material prepared by comparative example 1, the properties of embodiment 1 is all higher than comparative example 1, especially both abrasion of rolling are with the biggest gap, illustrate that composite lubricated low friction compound has self-lubricating and reduces the effect of friction, composite strengthening anti-wear agent not only has the effect reducing abrasion of rolling, and can also keep the mechanical property of matrix material; (3) method of matrix material prepared by comparative example 2 is traditional twin screw extrusion by melting, embodiment 1 is the dipping coating equipment adopting continuous fiber reinforced thermoplastic material, obtained tool height self lubricity and wear resistance and have in the high temperature resistant nylon composite material particle of high strength and thermotolerance, roving glass fiber is arranged in parallel with each other along composite material granular length direction, and length is identical with composite material granular length, the properties of embodiment 1 is all high than comparative example 1 a lot.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. continuous long fiber strengthens a high temperature resistant nylon composite material, it is characterized in that: be made up of the component comprising following weight part:
2. continuous long fiber according to claim 1 strengthens high temperature resistant nylon composite material, it is characterized in that: described high temperature resistant nylon resin be selected from fusing point be in semi-aromatic nylon between 290-330 DEG C or aromatic nylon one or more;
Preferably, described semi-aromatic nylon is the Alkylenediamine polycondensation of terephthalic acid or m-phthalic acid and 4-12 carbon atom and obtains; Described aromatic nylon is terephthalic acid or a toluene dioctyl phthalate and Ursol D or mphenylenediamine polycondensation and obtains;
Or described continuous fortifying fibre is one or more in continuous long glass fiber, continuous long basalt fibre, continuous long carbon fiber or continuous long aramid fiber, Fibre diameter is 9-13 μm.
3. continuous long fiber according to claim 1 strengthens high temperature resistant nylon composite material, it is characterized in that: described bismaleimides is diphenyl methane dimaleimide;
Or described compatilizer A is one or more in high-density polycthylene grafted maleic anhydride or high-density polycthylene grafted glycidyl methacrylate;
Or described compatilizer B is tetrabromo-bisphenol type epoxy resin.
4. continuous long fiber according to claim 1 strengthens high temperature resistant nylon composite material, it is characterized in that: described composite strengthening anti-wear agent is made up of the potassium titanate crystal whisker of the hollow glass micropearl of 5-25 part, the nano silicon of 1-6 part and 5-15 part.
5. continuous long fiber according to claim 4 strengthens high temperature resistant nylon composite material, it is characterized in that: the particle diameter of described hollow glass micropearl is 10-24 μm, and tap density is 0.8-1.6g/cm
3;
Or the median size of described nano silicon is 30nm, specific surface area is 600m
2/ g, loose density is 0.08g/cm
3, real density is 2.2g/cm
3;
Or described potassium titanate crystal whisker diameter is 0.1-0.5 μm, length 3-15 μm.
6. continuous long fiber according to claim 1 strengthens high temperature resistant nylon composite material, it is characterized in that: described composite lubricated low friction compound is made up of the tetrafluoroethylene of 5-15 part and the ultrahigh molecular weight polyethylene(UHMWPE) of 5-25 part; Preferably, described ultrahigh molecular weight polyethylene(UHMWPE) molecular weight is greater than 1,500,000.
7. continuous long fiber according to claim 4 strengthens high temperature resistant nylon composite material, it is characterized in that: described processing aid is made up of the oxidation inhibitor of 0.5-1.5 part and the lubricant of 0.5-3.5 part;
Preferably, described oxidation inhibitor is β-(3,5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, N, N'-is two-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine or three [2.4-di-tert-butyl-phenyl] phosphorous acid ester in one or more;
Or described lubricant is one or more in ultra-high molecular weight polysiloxane or pentaerythritol stearate.
8. continuous long fiber according to claim 1 strengthens high temperature resistant nylon composite material, it is characterized in that: described solidifying agent is one or more in mphenylenediamine, m-xylene diamine or quadrol;
Or in described continuous fiber enhancing high temperature resistant nylon composite material, fiber is arranged in parallel with each other along composite material granular length direction, and length is identical with composite material granular length.
9. in claim 1-8, arbitrary described continuous fiber strengthens a preparation method for high temperature resistant nylon composite material, it is characterized in that: comprise the following steps:
(1) by high temperature resistant nylon resin, compatilizer A, composite strengthening anti-wear agent, composite lubricated low friction compound difference, drying;
(2) each component raw material of following weight part is taken: 100 parts of high temperature resistant nylon resins, 5-15 part compatilizer A, 1-15 part bismaleimides, 11-46 part composite strengthening anti-wear agent, the composite lubricated low friction compound of 10-40 part, 1.0-5.0 part processing aid and 0.1-0.5 part solidifying agent, join in high-speed mixer successively and mix, mixing time is 5-15 minute; By the material mixed, it is mixing to add twin screw extruder upstream addition mouth; Synchronously carry out the process of compatilizer B surface impregnation to 35-155 part continuous fiber, the compatilizer B be impregnated on continuous fibre is 1-3 part;
(3) continuous fiber synchronous for compatilizer B surface impregnation in (2) is added long fine coating machine die head, carry out infiltration coated, fibre content is adjusted to 35-155 part, continuous fortifying fibre surface impregnation 1-3 part compatilizer B by the engine speed of twin screw extruder and feeding frequency; Through cooling, traction, pelletizing, obtain continuous fiber and strengthen high temperature resistant nylon composite material.
10. preparation method according to claim 9, is characterized in that: in described step (1), and high temperature resistant nylon raw material being placed in temperature is 110 DEG C of loft drier, dry 10h; Compatilizer A, composite strengthening anti-wear agent and composite lubricated low friction compound are placed in 80 DEG C of loft drier respectively, dry 4h;
Or in described step (2), the engine speed of twin screw extruder is that 200-300 turns/min, and feeding frequency is 15-35Hz.The length being 4-6m/min control pellet by the pulling speed of adjustment dicing machine is 11-13mm, and the diameter being controlled pellet by the size 2.5mm of sizing mouth mould is 2.5mm;
In described step (2), the temperature of twin screw extruder is set as 275-335 DEG C.
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Application publication date: 20150701 |