CN101182388B - High-wearing high-rigidity reinforced nylon 66 complexes and method for making same - Google Patents
High-wearing high-rigidity reinforced nylon 66 complexes and method for making same Download PDFInfo
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- CN101182388B CN101182388B CN2007101720739A CN200710172073A CN101182388B CN 101182388 B CN101182388 B CN 101182388B CN 2007101720739 A CN2007101720739 A CN 2007101720739A CN 200710172073 A CN200710172073 A CN 200710172073A CN 101182388 B CN101182388 B CN 101182388B
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Abstract
The invention relates to a highly wear-resistant and high-rigidity reinforced nylon 66 compound. The invention is characterized in that the compound consists of materials of the following weight portions: 66 portions to 100 portions of nylon, 0.1 portions to 15 portions of nucleater, 5 portions to 30 portions of wear-resistant agent, 0.5 portion to 3 portions of heat stabilizer and processing aid, and 15 portions to 105 portions of glass fiber. The invention has the advantage that each index all reaches or surpasses the scheduled requirements; the bending modulus of the material reach above 11000MPa; the hardness reaches to 135 N/mm2. Under the condition of no lubrication, surface pressure of 1.5 kg/m2, speed of 29 m/min and a temperature of 23 DEG C, the maximum static friction coefficient is 0.11; the maximum dynamic friction coefficient is 0.07. Under the condition of no lubrication, surface pressure of 100kg/cm<2> and speed of 23m/min, the PV value reaches above 2270kg/cm<2>. m/min.
Description
Technical field
The present invention relates to a kind of high-wearing high-rigidity reinforced nylon dragon 66 mixtures and preparation method thereof, be mainly used in the component that bearing, gear, lining, cylinder and cam etc. in the industries such as automobile, OA have relative movement, belong to the modified polyamide technical field.
Background technology
Nylon 66 is a kind of broad-spectrum engineering plastics, is formed by hexanediamine and hexanodioic acid polycondensation, and its fusing point is 246-263 ℃, and theoretical fusing point is 259 ℃ (DSC methods), and the second-order transition temperature under the dry state is 50 ℃.And the amide group on its molecular chain has polarity, easily forms hydrogen bond, thus its mechanical property excellence, as high strength, high-modulus, high rigidity etc.; Thermal characteristics is also very high, as thermal distortion, can reach 260 ℃ (load is 0.45MPa) after adding glass, 250 ℃ (load is 1.82MPa); Show excellent creep resistance, wear resistance and noise reduction etc. in addition.But also, make its water-absorbent height, cause its poor dimensional stability, thereby its wear resistance and thermotolerance are descended owing to itself this special structure.By general enhancing, the filling way can be improved its deficiency, and its performance is improved greatly.
General glass fiber reinforced nylon 66 existing market sales volumes are a lot, and there is very big-difference in the glass fiber reinforced nylon 66 that different manufacturers produces, general external manufacturer such as Dupont on performance, Asahi, Lanxess, BASF, Solutia, Dow chemical etc. have different grades, according to actual needs as high rigidity, high heat-resisting, anti-aging, anti-hydrolysis or the like, but also do not have high-wearing high-rigidity reinforced nylon dragon 66 mixtures.
Summary of the invention
The purpose of this invention is to provide a kind of high-wearing high-rigidity reinforced nylon dragon 66 mixtures and preparation method thereof.
For realizing above purpose, technical scheme of the present invention provides a kind of high-wearing high-rigidity reinforced nylon dragon 66 mixtures, it is characterized in that, is made up of following weight part raw material:
66 100 parts of nylon,
0.1 part-15 parts of nucleators,
5 parts-30 parts of anti-wear agents,
0.5 part-3 parts of thermo-stabilizer and processing aids,
15 parts-105 parts in glass fibre;
Described nucleator is a fusing point greater than 285 ℃ high molecular polymer, is linear polyphenylthioether PPS, oligopolymer hexanolactam dimer, PA46, all aromatic polyimide or PPA;
Said thermo-stabilizer and processing aid are phenols and phosphorous acid esters.
Described anti-wear agent is tetrafluoroethylene powder and graphite; Described glass fibre is a silane coupling agent, is stearic acid, stearate and alkyl sodium sulfonate;
Described phenols is four (β-(3, the 5-di-tert-butyl-hydroxy phenyl) pentaerythritol ester propionic acid), triglycol is two-3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester, β-(4-hydroxyl-3, the 5-di-tert-butyl-phenyl) the positive octadecanol ester of propionic acid, (2,4,6-trioxy--1,3,5-triazine-1,3,5 (2H, 4H, 6H)-three base) trivinyl three (3-(3, the 5-di-tert-butyl-hydroxy phenyl) acrylate), 2,2 '-thiobis (3-(3, the 5-di-tert-butyl-hydroxy phenyl) ethyl propionate), 3,5-two (1, the 1-dimethyl ethyl)-4-hydroxy phenylpropionic acid 2-(3-(3,5-two (1, the 1-dimethyl ethyl)-4-hydroxy phenyl)-1-oxopropyl) hydrazides; Described phosphorous acid esters are: tetramethylolmethane diphosphite two (2,4-di-tert-butyl phenyl) ester, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester, four (2,4-di-tert-butyl-phenyl-4,4 ' xenyl) biphosphonate, (18) ester, Tyox B on distearyl pentaerythritol diphosphite, the thio-2 acid.
A kind of preparation method of high-wearing high-rigidity reinforced nylon dragon 66 mixtures is characterized in that, the steps include:
The first step. take by weighing raw material by weight;
Second step. PA66 resin, nucleator, anti-wear agent, thermo-stabilizer and processing aid is even in high-speed mixer and mixing, and mixing time is 90 seconds-150 seconds;
The 3rd step. mixed raw materials is entered into the twin screw extruder of specifying screw combinations, under 220-350 ℃ temperature,, promptly obtain high rigidity high abrasion Reinforced Nylon 66 mixtures of the present invention with the mixing extruding pelletization of glass fibre.
The present invention adopts nucleator in glass fiber reinforced nylon 66, makes it the spherocrystal refinement, and fusing point, rigidity, surface hardness, surface gloss and dimensional stability obtain to increase substantially, and simultaneously, the toughness loss is also very little.Glass fibre has the active characteristics of hydrophobic group low surface energy.
Advantage of the present invention is that every index all meets or exceeds pre-provisioning request, and the modulus in flexure of material is reached more than the 11000MPa, and hardness reaches 135N/mm
2. unlubricated, surface pressure 1.5kg/m
2, speed is under 29m/min, 23 ℃ of conditions of temperature, coefficient of maximum static friction 0.11, maximum kinetic friction coefficient 0.07; At unlubricated, surface pressure is 100kg/cm
2, speed is under the 23m/min condition, the PV value reaches 2270kg/cm
2.m/min more than.
Embodiment
The invention will be further described below in conjunction with embodiment.
The major equipment of producing this mixture employing has:
High-speed mixer: rotating speed 450-1300 rev/min;
Twin screw extruder: screw speed 350-450rpm, barrel zone temperature are 220-350 ℃;
Tank: water temperature 20-40 ℃; Dicing machine: rotating speed 400-700rpm.
Embodiment 1
It is 2.7 ± 0.02 PA6621SPC that nylon 66 is selected the limiting viscosity of DOW chemistry for use;
It is the line style PPSRyton R-6 of 4-5 ten thousand that nucleator is selected the weight-average molecular weight of U.S. Phillips Petroleum for use;
The polytetrafluorethylepowder powder PTFE that anti-wear agent selects for use Shanghai fluoroplastics institute to produce;
Glass fibre is selected the glass fibre Saint go bain 983 that handles certainly of U.S. Saint go bain for use;
Thermo-stabilizer and processing aid are selected for use and are Ciba (N, N '-1,6-dihexyl two (3,5-two (1, the 1-dimethyl ethyl)-4-hydroxybenzene propionyl, tetramethylolmethane diphosphite two (2,4-di-tert-butyl phenyl) ester).
With limiting viscosity is that 2.7 ± 0.02 PA66 100kg, the polymerization degree are that line style PPS 10kg, anti-wear agent polytetrafluorethylepowder powder PTFE (M1300 Shanghai fluoroplastics institute) 10kg, thermo-stabilizer and processing aid 0.9kg put into high mixer and be mixed under the 450rpm condition, join in the twin screw extruder mixing, at glass fibre inlet apart from main spout 950mm place, the 52kg glass fibre joined be full of in the good melt extruder of plasticizing, it is cut off and melt thorough mixing, infiltration, dispersion, extrude pelletizing through head.Melt extruding temperature is 240-320 ℃, the temperature of each section is followed successively by: 240 ± 10 ℃, and 250 ± 10 ℃, 260 ± 10 ℃, 270 ± 10 ℃, 280 ± 10 ℃, 280 ± 10 ℃, 270 ± 10 ℃, 260 ± 10 ℃, 260 ± 10 ℃, 270 ± 10 ℃, promptly obtain high-wearing high-rigidity reinforced nylon dragon 66 mixtures of the present invention.
The thermal distortion of high-molecular linear polyphenyl thioether PPS is 260 ℃ (1.82MPa), and the life-time service temperature is 200-240 ℃.Below 204 ℃, be insoluble in all solvents, be not subjected to the corrosion of general soda acid; Under the high temperature its mechanical properties decrease seldom, resistance to fatigue, creep resistance and inherent flame retardant resistance are splendid.Its size is almost constant under hot and humid environment; Under 240 ℃ of high temperature, still can keep fine wear resistance.And form hydrogen bond between c h bond on amide group and the PPS phenyl ring on the PA66 molecule, make PPS and PA66 form extraordinary nucleocapsid structure; Because PPS has the thermofixation crosslinking feature in air,, can form the semiinterpenetrating polymer network transition layer at PA66 and PPS interface, thereby strengthen the two-phase interface bonding force greatly simultaneously with the PA66 blend.
Because PPS and PA66 interface easily form very strong bonding force, and the two has " S-" and amide group " NH-CO-" respectively, very easily with the active coupling agent generation chemical reaction on glass surface, make the three form an aggregate closely, intensity, rigidity, surface hardness and the water resistance of material are increased substantially.
Product of the present invention can adopt iso standard, detects.Test sample, by CJ80NC type injection moulding machine 240-350 ℃ of following injection moulding.
The measuring mechanical property method:
1. tensile strength: press ISO 527-2 test;
Pulling experiment machine model: LJ-1000 speed: 10mm/min
2. flexural strength: press ISO 178 tests;
Pulling experiment machine model: LJ-1000 speed: 2mm/min;
3. thermal change type temperature: press ISO 75-2 test;
4. proportion: press ISO 1183 tests;
5. content of glass fiber: press ISO 3451/1 test;
6. frictional coefficient: press ISO 8295 tests:
7. frictional wear amount limit PV value: press ISO 6601 tests;
8. hardness: press ISO 2039-2 test;
9. surface gloss: press ISO 2813 tests
Above-mentioned mixture is detected its result such as following table:
| Performance | Testing method | Unit | Embodiment 1 |
| Proportion | ISO1183 | g/cm 3 | 1.361 |
| Rockwell hardness | ISO2039-2 | R?Scale | 132 |
| Surface gloss | ISO2813 | -- | 95 |
| Stretching hardness | ISO527-2 | MPa | 205 |
| Flexural strength | ISO178 | MPa | 320 |
| Modulus in flexure | ISO178 | MPa | 11500 |
Annotate: measuring friction coefficient condition: unlubricated, surface pressure 1.5kg/m
2, 23 ℃ of speed 29m/min, temperature, frictional wear limit PV value condition determination: unlubricated, surface pressure is 100kg/cm
2, speed is 23m/min
Embodiment 2
It is 2.7 ± 0.02 PA66 21SPC that nylon 66 is selected the limiting viscosity of DOW chemistry for use;
Nucleator is selected the fully aromatic polyamide PPA of U.S. Du Pont company for use;
The polytetrafluorethylepowder powder PTFE that anti-wear agent selects for use Shanghai fluoroplastics institute to produce;
Glass fibre is selected the glass fibre Saint go bain 983 that handles certainly of U.S. Saint go bain for use;
Thermo-stabilizer and processing aid are selected CibaN for use, N '-1,6-dihexyl two (3,5-two (1, the 1-dimethyl ethyl)-4-hydroxybenzene propionyl and tetramethylolmethane diphosphite two (2,4-di-tert-butyl phenyl) ester.
With limiting viscosity 2.7 ± 0.02 PA66 100kg, fully aromatic polyamide PPA 10KG, anti-wear agent polytetrafluorethylepowder powder PTFE 10KG (M1300 Shanghai fluoroplastics institute), thermo-stabilizer and processing aid 0.9KG put into high mixer and mix under the 450rpm condition, join in the twin screw extruder mixing, add the 52KG glass fibre to being full of in the good melt extruder of plasticizing at glass mouth apart from main spout 950mm place, it is cut off and the melt thorough mixing, soak into, disperse, extrude pelletizing through head, melt extruding temperature is 240-350 ℃, and each section temperature is followed successively by: 240 ± 10 ℃, 250 ± 10 ℃, 260 ± 10 ℃, 270 ± 10 ℃, 280 ± 10 ℃, 280 ± 10 ℃, 270 ± 10 ℃, 260 ± 10 ℃, 260 ± 10 ℃, 270 ± 10 ℃, promptly obtain high-wearing high-rigidity reinforced nylon dragon 66 mixtures of the present invention.
This all aromatic polyimide selects PPA (DUPONT), and its fusing point is 345 ℃, and second-order transition temperature is 275 ℃, stretching property is very good by force for it, and long-term hot-air aging resistance is good, and dimensional stability is good, wear resistance is good, and is good with the PA66 intermiscibility, is the extraordinary nucleator of PA66.
Above-mentioned product is detected its result such as following table:
| Performance | Testing method | Unit | Embodiment 2 |
| Proportion | ISO1183 | g/cm 3 | 1.36 |
Subordinate list one:
Various glass fiber reinforced nylon 6s 6 are from the frictional coefficient of combination
(condition: unlubricated, surface pressure 1.4kg/cm
2, speed 29m/min, 25 ℃ of temperature)
Subordinate list two:
Various glass fiber reinforced nylon 6s 6 are from the limit PV value of combined friction wearing and tearing
(condition: unlubricated, surface pressure 100kg/cm
2, speed 23m/min)
Claims (3)
1. high-wearing high-rigidity reinforced nylon dragon 66 mixtures is characterized in that, are made up of following weight part raw material:
66 100 parts of nylon,
0.1 part-15 parts of nucleators,
5 parts-30 parts of anti-wear agents,
0.5 part-3 parts of thermo-stabilizer and processing aids,
15 parts-105 parts in glass fibre;
Described nucleator is a fusing point greater than 285 ℃ high molecular polymer, is linear polyphenylthioether PPS, oligopolymer hexanolactam dimer, PA46, all aromatic polyimide or PPA;
Said thermo-stabilizer and processing aid are phenols and phosphorous acid esters.
2. according to said a kind of high-wearing high-rigidity reinforced nylon dragon 66 mixtures of claim 1, it is characterized in that said phenols is four (β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester, triglycol is two-3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester, β-(4-hydroxyl-3, the 5-di-tert-butyl-phenyl) the positive octadecanol ester of propionic acid, (2,4,6-trioxy--1,3,5-triazine-1,3,5 (2H, 4H, 6H)-three base) trivinyl three (3-(3, the 5-di-tert-butyl-hydroxy phenyl) acrylate), 2,2 '-thiobis (3-(3, the 5-di-tert-butyl-hydroxy phenyl) ethyl propionate), 3,5-two (1, the 1-dimethyl ethyl)-4-hydroxy phenylpropionic acid 2-(3-(3,5-two (1, the 1-dimethyl ethyl)-4-hydroxy phenyl)-1-oxopropyl) hydrazides.
3. according to said a kind of high-wearing high-rigidity reinforced nylon dragon 66 mixtures of claim 1, it is characterized in that, said phosphorous acid esters are tetramethylolmethane diphosphite two (2,4-di-tert-butyl phenyl) ester, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester, four (2,4-di-tert-butyl-phenyl-4,4 ' xenyl) biphosphonate, (18) ester, Tyox B on distearyl pentaerythritol diphosphite, the thio-2 acid.
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| CN2007101720739A CN101182388B (en) | 2007-12-11 | 2007-12-11 | High-wearing high-rigidity reinforced nylon 66 complexes and method for making same |
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| CN101182388B true CN101182388B (en) | 2011-04-20 |
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| CN110964317A (en) * | 2019-10-30 | 2020-04-07 | 南京聚隆科技股份有限公司 | High-wear-resistance high-dimensional-stability steering turbine material and preparation method thereof |
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Address after: 201714 No. 88, Kang Yuan Garden, Zhujiajue Industrial Zone, Qingpu District, Shanghai Patentee after: Shanghai Kingfa Science and Technology Development Co., Ltd. Patentee after: Kingfa Technology Co., Ltd. Address before: 201714 No. 88 Kang Yuan Road, Zhujiajue Industrial Zone, Qingpu District, Shanghai Patentee before: Shanghai Kingfa Science and Technology Development Co., Ltd. Patentee before: Guangzhou Jinfa Science & Technology Co., Ltd. |