CN107446346A - A kind of wear-resisting high-temperature nylon composite of fibre reinforced and preparation method thereof - Google Patents
A kind of wear-resisting high-temperature nylon composite of fibre reinforced and preparation method thereof Download PDFInfo
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Abstract
A kind of wear-resisting high-temperature nylon composite of fibre reinforced, include the component of following parts by weight:High-temperature nylon resin 35% 85%, carbon fiber 5% 45%, complex abrasion-proof auxiliary agent 5% 20%, antioxidant 0.2% 0.6%, the complex abrasion-proof auxiliary agent is to be made up of through coupling agent modified mixed fillers, the mixed fillers the soft filler and the hard filler of Mohs' hardness >=5 of Mohs' hardness≤2.The wear-resisting high-temperature nylon composite of fibre reinforced of the present invention also has low abrasion amount, excellent combination property while having mechanical property, heat resistance, low-friction coefficient concurrently in high-mechanic.
Description
Technical field
The invention belongs to high-temperature nylon material technical field, more particularly to a kind of nylon composite materials and preparation method thereof.
Background technology
High-temperature nylon resin refers generally to nylon engineering plastic of the modified long-term use of temperature more than 150 DEG C, at present work
The major product of industry includes amorphous nylon PA46 and semi-aromatic nylon PA4T, PA6T, PA9T and PA10T etc..High temperature Buddhist nun
Imperial resin has the advantages that good mechanical performance, wearability, heat resistance and the chemically-resistant property of medicine, semi-aromatic high-temperature nylon resin
Also overcome the shortcomings that nylon resin water absorption rate is high.High-temperature nylon resin can be used for sliding part and the structures such as gear, bearing, valve
Part, fuel conduit etc., but if using unmodified high-temperature nylon resin as high-abrasive material, especially lubricating condition compared with
Under poor or larger load working condition, its bearing capacity is inadequate, and self lubricity is poor, and wear extent is big in high-speed friction, it is difficult to
Meet the requirement of the self-lubricating structural timber for a long time with surface abrasion resistance damage and low frictional property under high loads.One
As for, addition carbon fiber and antiwear assistant can lift the performance of nylon resin.
Carbon fiber is high strength and modulus fiber of the phosphorus content more than 90%, is with a kind of strengthening material of excellent performance
Material.Carbon fiber and carbon fibre composite have high intensity, high-modulus, high temperature resistant, light weight, wear-resisting, creep resistant and thermal expansion
The advantages such as coefficient is low, are widely used in field of compound material.But carbon fiber surface is in chemical inertness, with thermoplastic
Compatibility is poor between property resin matrix, and carbon fiber is difficult to, with matrix resin Nian Jie poor, shadow dispersed in matrix resin difficulty
Ring the performance of composite material combination property.
The selection of antiwear assistant to improve high-abrasive material coefficient of friction and reduce high-abrasive material wear extent suffer to
Close important effect.It is generally acknowledged that the filler of soft, particularly Mohs' hardness be less than 2 filler, as graphite, molybdenum disulfide,
Talcum, mica and ptfe micropowder etc., abrasion of the coefficient of friction and can reduction of material to mating material can be reduced.But
Under larger load, when these high-abrasive materials occur to rub with respect to slip with the bigger mating material of hardness, part can be caused
Overheat, causes high temperature, and high-abrasive material can form adhesive wear because high temperature softens and is sheared and comes off.
Patent document CN101343409B discloses a kind of fibre reinforced thermoplas tic resin composite, using through surface
The thermoplastics such as carbon fiber reinforced nylon, makrolon, PET, polypropylene and ABS after processing, and
Polytetrafluoroethylene (PTFE) is added to lower coefficient of friction, but the patent fails to solve the problems, such as that material abrasion is excessive during high-mechanic.
Patent document CN104744926A discloses a kind of continuous long fiber enhancing high temperature resistant nylon composite material, including following
Component and parts by weight:It is 100 parts of high temperature resistant nylon resin, continuous reinforcing fiber 35-155 parts, BMI 1-15 parts, compatible
Agent A5-15 parts, compatilizer B1-3 parts, composite strengthening antiwear additive 11-46 parts, composite lubricated anti-friction agent 10-40 parts, processing aid
1.0-5.0 part and curing agent 0.1-0.5 parts.The patent system possesses mechanics for continuous fiber enhancing high temperature resistant nylon composite material
Performance, heat-resisting quantity and dimensional stability, but fibre length is big in continuous long fiber enhancing high temperature resistant nylon composite material, is unfavorable for
The coefficient of friction of material and the reduction of abrasion, while continuous long fiber enhancing high temperature resistant nylon composite material needs to have former
Particular/special requirement, complex process.
The content of the invention
The technical problems to be solved by the invention are to overcome the shortcomings of to mention in background above technology and defect, there is provided a kind of
The also fibre reinforced with low abrasion amount is resistance to while having mechanical property, heat resistance, low-friction coefficient concurrently in high-mechanic
High-temperature nylon composite is ground, and its preparation method is accordingly provided.In order to solve the above technical problems, technical side proposed by the present invention
Case is:
A kind of wear-resisting high-temperature nylon composite of fibre reinforced, include the component of following parts by weight:High-temperature nylon resin
35%-85%, carbon fiber 5%-45%, complex abrasion-proof auxiliary agent 5%-20%, antioxidant 0.2%-0.6%, the complex abrasion-proof
Auxiliary agent is soft filler and Mohs' hardness >=5 of the mixed fillers by Mohs' hardness≤2 through coupling agent modified mixed fillers
Hard filler form.
In the above-mentioned wear-resisting high-temperature nylon composite of fibre reinforced, it is preferred that the soft filler and hard filler
Mass ratio is 3:1-9:1, the quality of the coupling agent is the soft filler and the 0.3%- of the quality summation of hard filler
1%.
Inventor has found that the coefficient of friction and can that material can be reduced using single soft filler is subtracted in research process
Few abrasion to mating material, but under larger load, these high-abrasive materials occur relatively sliding with the bigger mating material of hardness
When moving and rubbing, hot-spot can be caused, causes high temperature, high-abrasive material can be formed glutinous because high temperature soften and be sheared and come off
Abrasion.But inventor has found to use mass ratio as 3:1-9:The mixed fillers of 1 soft filler and hard filler, warp
After coupling agent treatment, can solve the problems, such as that above-mentioned wear extent is big.Because in mixed fillers after coupling agent treatment
Soft filler can form stabilization, continuous and smooth transfer membrane in friction process in frictional interface, can effectively reduce wear-resisting material
The coefficient of friction and wear extent of material;Hard filler in mixed fillers can improve the modulus, hardness and heat resistance of high-abrasive material,
Friction process mainly plays carrying, and mitigation is sticked together, and prevents the extension and pyroplastic deformation and softening of ditch dug with a plow, reduces material
Wear extent, thus add mixed fillers after coupling agent treatment effectively to alleviate high-abrasive material bigger with hardness under heavy load
Mating material occur rubbed with respect to slip produce adhesive wear, wear extent can be reduced.But hard filler should not be excessive, no
The coefficient of friction of composite can then be increased, be unfavorable for the raising of composite material combination property.
In the above-mentioned wear-resisting high-temperature nylon composite of fibre reinforced, it is preferred that the soft filler is graphite, curing
One or more in molybdenum, talcum, mica and ptfe micropowder, the hard filler are wollastonite, aluminum oxide and carbonization
One or more in silicon.
In the above-mentioned wear-resisting high-temperature nylon composite of fibre reinforced, it is preferred that the coupling agent be titanate coupling agent,
One or more in aluminate coupling agent and zirconium ester coupling agent.
In the above-mentioned wear-resisting high-temperature nylon composite of fibre reinforced, it is preferred that the high-temperature nylon resin is that fusing point exists
The one or more in semi-aromatic nylon resin or semi-aromatic nylon resin copolymer between 280 DEG C -330 DEG C.Such as
The optional carbon diamines (PA13T) of autohemagglutination paraphenylene terephthalamide 13, the carbon diamines (PA11T) of poly- paraphenylene terephthalamide 11, poly- terephthaldehyde
The carbon diamines (PA12T) of acyl 12, poly- hexamethylene terephthalamide-co- polycaprolactam co-polymers (PA6T/6), poly- terephthaldehyde
Acyl hexamethylene diamine-co- polyhexamethylene adipamide copolymer (PA6T/66), the poly- paraphenylene terephthalamides of poly-paraphenylene terephthalamide's nonamethylene diamine-co-
Decamethylene diamine copolymer (PA9T/10T).Composite can produce substantial amounts of heat, poor heat resistance under the friction duty of high-voltage high-speed
Material easily soften, be quickly worn.Above-mentioned matrix resin, have good wearability, heat resistance and the chemically-resistant property of medicine and
Mechanical performance, the use condition of the bad working environments such as high-mechanic, high temperature and insufficient lubrication can be met.
In the above-mentioned wear-resisting high-temperature nylon composite of fibre reinforced, it is preferred that the carbon fiber is through nitric acid Oxygen in Liquid
PAN base milled carbon fibers after the processing of change method, the filament diameter of the PAN bases milled carbon fiber is 5-8 μm, average fiber length
For 50 μm -200 μm.Milled carbon fiber has the advantages that distribution of lengths is uniform, and dispersiveness is excellent, can effectively improve carbon fiber in base
Scattering problem in body resin, the mechanical property and frictional behaviour of material are improved, can be carried using preceding progress liquid phase oxidation processing
Its high bonding force with high-temperature nylon resin, modified effect are more excellent.
In the above-mentioned wear-resisting high-temperature nylon composite of fibre reinforced, it is preferred that the antioxidant is N, N- is double-(3- (3,
5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine and three (2,4- tert-butyl-phenyls) phosphite esters are by weight being 0.5:
1-2:1 mixed mixture.
The technical concept total as one, the present invention also provide a kind of wear-resisting high-temperature nylon composite of fibre reinforced
Preparation method, comprise the following steps:
(1) soft filler is dried with hard filler and is well mixed to obtain mixed fillers, it is under agitation that coupling agent is molten
Liquid is sprayed on mixed fillers surface, and re-dry obtains complex abrasion-proof auxiliary agent;
(2) carbon fiber is put into salpeter solution and heated, then washing and drying obtains the carbon fiber through liquid phase oxidation;
(3) high-temperature nylon resin is dried, then by high-temperature nylon resin, complex abrasion-proof auxiliary agent, antioxidant it is well mixed after
Being added from the main spout of screw extruder, carbon fiber adds from screw extruder side spout, is extruded after melting, through cooling down,
Pelletizing, obtain the wear-resisting high-temperature nylon composite of fibre reinforced after drying.
In the preparation method of the above-mentioned wear-resisting high-temperature nylon composite of fibre reinforced, it is preferred that the coupling agent solution
For coupling agent is added in isopropanol, and keep 10-30 times that isopropanol quality is coupling agent quality.Isopropanol also can use fusing point
Substituted for 60-85 DEG C of alcohols solvent, but preferably isopropanol.
In the preparation method of the above-mentioned wear-resisting high-temperature nylon composite of fibre reinforced, it is preferred that the salpeter solution
Mass fraction is 30%-65%, and the condition of the heating is to heat 0.5-3h in 60 DEG C of -80 DEG C of water-baths.
Specifically, the step of preparation method of the above-mentioned wear-resisting high-temperature nylon composite of fibre reinforced, is as follows:
(1) soft filler and hard filler are placed in electric drying oven with forced convection, mixed after 6-8h is dried at 80-120 DEG C
Conjunction uniformly obtains mixed fillers, and coupling agent is dissolved in isopropanol and is configured to coupling agent solution, and keeps isopropanol quality as occasionally
Join 10-30 times of agent quality, then mixed fillers are placed in mixer and stirred, be sprayed at coupling agent solution in whipping process mixed
The surface of filler is closed, mixing time 10-20min, the mixed fillers for spraying coupling agent solution is finally placed in electric heating air blast and done
In dry case, 3-6h is dried at 80-100 DEG C, obtains the complex abrasion-proof auxiliary agent;
(2) carbon fiber is put into the nitric acid that mass fraction is 30%-65%, 0.5- is heated in 60 DEG C of -80 DEG C of water-baths
After 3h, with carbon fiber of the distilled water flushing after nitric acid treatment until the pH value of distilled water is 7 or so, finally carbon fiber is put into
In baking oven, 8-12h is dried at 75 DEG C -85 DEG C, obtains the carbon fiber through liquid phase oxidation;
(3) high-temperature nylon resin is put into baking oven, dries 4-6h at 110-130 DEG C, then by high-temperature nylon resin, multiple
Close antiwear assistant, antioxidant to be well mixed in high-speed mixer, added from the main spout of screw extruder, by carbon fiber from
The side spout of screw extruder adds, and it is 290 DEG C -335 DEG C to keep extrusion temperature, screw speed 200r/min-500r/
Min, extruded after melting, the wear-resisting high-temperature nylon composite of fibre reinforced is obtained after cooling, pelletizing, drying.
Compared with prior art, the advantage of the invention is that:
1st, the present invention use matrix resin of the high temperature resistant nylon resin as composite, with good wearability, resistance to
Hot and the chemically-resistant property of medicine and mechanical performance, the use condition of the bad working environments such as high-mechanic, high temperature and insufficient lubrication can be met.
2nd, complex abrasion-proof auxiliary agent of the invention, the high-abrasive material antithesis material bigger with hardness under heavy load can effectively be alleviated
The caused adhesive wear that rubbed with respect to slip occurs for material, reduces wear extent.In addition, antiwear assistant after coupling agent treatment with base
The adhesion of body resin significantly improves, and can improve the mechanical property of material.
3rd, high temperature resistant nylon resin, complex abrasion-proof auxiliary agent and carbon fiber three have complementary advantages in the present invention, are prepared
The wear-resisting high-temperature nylon composite of fibre reinforced had concurrently in high-mechanic mechanical property, heat resistance, low-friction coefficient it is same
When also there is low abrasion amount, excellent combination property.
Embodiment
For the ease of understanding the present invention, more comprehensively, meticulously retouched below in conjunction with preferred embodiment to inventing to do herein
State, but protection scope of the present invention is not limited to specific examples below.
Unless otherwise defined, all technical terms used hereinafter are generally understood that implication phase with those skilled in the art
Together.Technical term used herein is intended merely to describe the purpose of specific embodiment, is not intended to the limitation present invention's
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
A kind of wear-resisting high-temperature nylon composite of fibre reinforced, its component and content are as shown in table 1 below, wherein, it is soft
Mohs' hardness≤2 of filler, Mohs' hardness >=5 of hard filler, carbon fiber are the PAN bases after the processing of nitric acid liquid phase oxidation
Milled carbon fiber, filament diameter of the PAN bases milled carbon fiber through nitric acid liquid phase oxidation before processing are 7 μm, average fiber length
For 100 μm.
The preparation method of the wear-resisting high-temperature nylon composite of this implementation fibre reinforced is as follows:
(1) soft filler and hard filler are placed in electric drying oven with forced convection, are well mixed after 8h is dried at 100 DEG C
Mixed fillers are obtained, coupling agent is dissolved in isopropanol and is configured to coupling agent solution, and it is coupling agent matter to keep isopropanol quality
20 times of amount, then mixed fillers are placed in mixer and stirred, coupling agent solution is sprayed at mixed fillers in whipping process
Surface, mixing time 15min, finally the mixed fillers for spraying coupling agent solution are placed in electric drying oven with forced convection, 90
4h is dried at DEG C, obtains the complex abrasion-proof auxiliary agent;
(2) carbon fiber is put into the nitric acid that mass fraction is 60%, after heating 1h in 70 DEG C of water-baths, rushed with distilled water
The carbon fiber washed after nitric acid treatment is 7 or so up to the pH value of distilled water, finally carbon fiber is put into baking oven, at 80 DEG C
10h is dried, obtains the carbon fiber through liquid phase oxidation;
(3) high-temperature nylon resin is put into baking oven, 6h is dried at 120 DEG C, then by high-temperature nylon resin, complex abrasion-proof
Auxiliary agent, antioxidant are well mixed in high-speed mixer, are added from the main spout of screw extruder, carbon fiber is squeezed from screw rod
The side spout for going out machine adds, and it is 300 DEG C to keep extrusion temperature, screw speed 400r/min, is extruded after melting, through cooling down,
Pelletizing, obtain the wear-resisting high-temperature nylon composite of fibre reinforced after drying.
The wear-resisting high-temperature nylon composite of fibre reinforced that the present embodiment is prepared carries out performance test, test knot
Fruit is as shown in table 1 below.
Embodiment 2-4:
A kind of wear-resisting high-temperature nylon composite of fibre reinforced, compared with Example 1, difference is in its constituent
Content it is different, specific difference see the table below 1.The preparation method of the present embodiment is same as Example 1.
Comparative example 1-3:
A kind of wear-resisting high-temperature nylon composite of fibre reinforced, compared with embodiment 1-4, difference its form into
The content divided is different, and specific difference see the table below 1.
Table 1:Embodiment 1-4 and comparative example 1-3 raw material and performance data
As seen from the above table, the combination property for the composite being prepared in embodiment 1-4 is substantially better than in comparative example 1-3
The composite being prepared, it is significantly superior especially to wear away this performance.
In upper table, tensile strength and modulus press GB/T 1040-2006 standard testings, tensile strength test rate 50mm/
Min, stretch modulus test rate 1mm/min;Bending strength and modulus press GB/T 9341-2008 standard testings, tensile strength and
Modulus test speed 2mm/min;Simply supported beam notch impact strength and unnotched impact strength are surveyed by GB/T1043-2008 standards
Examination, notch strength pendulum energy 1J, unnotched impact strength pendulum energy 7.5J;Heat distortion temperature is marked by GB/T 1643-2004
Quasi- test, 1.8MPa loads;Coefficient of friction and abrasion are tested by national standard GB/T 3960-2016, apply 1250N power, 45# steel pair
Bull ring, area 125mm2。
Claims (10)
1. a kind of wear-resisting high-temperature nylon composite of fibre reinforced, it is characterised in that include the component of following parts by weight:High temperature
Nylon resin 35%-85%, carbon fiber 5%-45%, complex abrasion-proof auxiliary agent 5%-20%, antioxidant 0.2%-0.6%, it is described
Complex abrasion-proof auxiliary agent be through coupling agent modified mixed fillers, the mixed fillers by Mohs' hardness≤2 soft filler with not
The hard filler of family name hardness >=5 is formed.
2. the wear-resisting high-temperature nylon composite of fibre reinforced according to claim 1, it is characterised in that described soft to fill out
The mass ratio of material and hard filler is 3:1-9:1, the quality of the coupling agent is the quality of the soft filler and hard filler
The 0.3%-1% of summation.
3. the wear-resisting high-temperature nylon composite of fibre reinforced according to claim 1 or 2, it is characterised in that described soft
Matter filler is the one or more in graphite, molybdenum disulfide, talcum, mica and ptfe micropowder, and the hard filler is
One or more in wollastonite, aluminum oxide and carborundum.
4. the wear-resisting high-temperature nylon composite of fibre reinforced according to claim 1 or 2, it is characterised in that the idol
Connection agent is the one or more in titanate coupling agent, aluminate coupling agent and zirconium ester coupling agent.
5. the wear-resisting high-temperature nylon composite of fibre reinforced according to claim 1 or 2, it is characterised in that the height
Warm nylon resin is fusing point in the semi-aromatic nylon resin or semi-aromatic nylon resin copolymer between 280 DEG C -330 DEG C
One or more.
6. the wear-resisting high-temperature nylon composite of fibre reinforced according to claim 1 or 2, it is characterised in that the carbon
Fiber is the PAN base milled carbon fibers after the processing of nitric acid liquid phase oxidation, and the filament diameter of the PAN bases milled carbon fiber is
5-8 μm, average fiber length is 50 μm -200 μm.
7. the wear-resisting high-temperature nylon composite of fibre reinforced according to claim 1 or 2, it is characterised in that described anti-
Oxygen agent is N, and N- pairs-(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine and three (2,4- tert-butyl-phenyls) are sub-
Phosphate is 0.5 by weight:1-2:1 mixed mixture.
A kind of 8. preparation side of the wear-resisting high-temperature nylon composite of fibre reinforced as any one of claim 1-7
Method, it is characterised in that comprise the following steps:
(1) soft filler is dried with hard filler and is well mixed to obtain mixed fillers, under agitation spray coupling agent solution
It is sprinkled upon on mixed fillers surface, re-dry obtains complex abrasion-proof auxiliary agent;
(2) carbon fiber is put into salpeter solution and heated, then washing and drying obtains the carbon fiber through liquid phase oxidation;
(3) high-temperature nylon resin is dried, then by high-temperature nylon resin, complex abrasion-proof auxiliary agent, antioxidant it is well mixed after from spiral shell
The main spout of bar extruder adds, and carbon fiber adds from screw extruder side spout, is extruded after melting, through cooling, pelletizing,
The wear-resisting high-temperature nylon composite of fibre reinforced is obtained after drying.
9. preparation method according to claim 8, it is characterised in that the coupling agent solution is that coupling agent is added into isopropyl
In alcohol, and keep 10-30 times that isopropanol quality is coupling agent quality.
10. preparation method according to claim 8, it is characterised in that the mass fraction of the salpeter solution is 30%-
65%, the condition of the heating is to heat 0.5-3h in 60 DEG C of -80 DEG C of water-baths.
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CN111849049A (en) * | 2019-04-28 | 2020-10-30 | 合肥杰事杰新材料股份有限公司 | Cold-resistant wear-resistant polyethylene composite material and preparation method thereof |
CN110483992A (en) * | 2019-09-04 | 2019-11-22 | 株洲时代新材料科技股份有限公司 | A kind of low warpage enhancing semi-aromatic high-temperature nylon composite material and preparation method |
CN110483992B (en) * | 2019-09-04 | 2021-11-16 | 株洲时代新材料科技股份有限公司 | Low-warpage reinforced semi-aromatic high-temperature nylon composite material and preparation method thereof |
CN111303629A (en) * | 2019-12-27 | 2020-06-19 | 长沙新材料产业研究院有限公司 | High-temperature-resistant self-lubricating wear-resistant composite material and preparation method thereof |
CN112480667A (en) * | 2020-12-18 | 2021-03-12 | 南京串晶科技有限公司 | Formula and preparation method of high-wear-resistance special nylon material |
CN112480666A (en) * | 2020-12-18 | 2021-03-12 | 南京串晶科技有限公司 | Formula and preparation method of high-wear-resistance modified PA9T composite material |
CN112644094A (en) * | 2020-12-22 | 2021-04-13 | 南京特塑复合材料有限公司 | High-temperature-resistant composite material shielding pipe |
CN113214601A (en) * | 2021-04-13 | 2021-08-06 | 句容市久诺复合材料有限公司 | Wear-resistant SMC (sheet molding compound) material synthesized by epoxy resin |
CN113429783A (en) * | 2021-07-09 | 2021-09-24 | 浙江谱奈图新材料科技有限公司 | Low-friction low-abrasion high-temperature nylon and preparation method thereof |
CN114163769A (en) * | 2021-12-09 | 2022-03-11 | 刘成龙 | Environment-friendly wear-resistant high polymer material and processing technology thereof |
CN115322560A (en) * | 2022-08-24 | 2022-11-11 | 湖北合聚新材料有限公司 | Wear-resistant nylon material and preparation method and application thereof |
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