CN103740102B - A kind of electric conduction nylon composite material and preparation method thereof - Google Patents
A kind of electric conduction nylon composite material and preparation method thereof Download PDFInfo
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- CN103740102B CN103740102B CN201310745328.1A CN201310745328A CN103740102B CN 103740102 B CN103740102 B CN 103740102B CN 201310745328 A CN201310745328 A CN 201310745328A CN 103740102 B CN103740102 B CN 103740102B
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- composite material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92561—Time, e.g. start, termination, duration or interruption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a kind of electric conduction nylon composite material and preparation method thereof.Electric conduction nylon composite material is the most composed of the following components: PA121282-90%；Graphene 1-5%；Antioxidant 0.1-1%；Coupling agent 0.5-1%；Toughener 8-13%；Silicone oil 0.5-1%.The coupling agent of the present invention can improve Graphene and resin compatible well. and the addition of toughener improves the toughness of material, and a small amount of Graphene just can accomplish conduction.The electric conduction nylon composite material conductivity height of the present invention, good toughness, preparation process are simple, and production technology is easily controlled.
Description
[technical field]
The present invention relates to polymeric material field, particularly relate to a kind of electric conduction nylon composite material and preparation method thereof.
[background technology]
The performance that long carbon chain nylon possesses has a more preferable dimensional stability than traditional PA6 and PA66, and superior resistance to
Chemical corrosivity, traditional conductive nylon material, it will usually add the conductive agent of some electrically conductive graphites or precipitation type, but
PA6 and PA66 to accomplish conduction, and not only the conductive agent addition of graphite or precipitation type is big, and to PA6 and PA66 material
Performance impact also big, particularly impact strength aspect can weaken a lot, and material can be highly brittle.
[summary of the invention]
The technical problem to be solved in the present invention is to provide a kind of has that conductivity is high, the electric conduction nylon composite material of good toughness
And preparation method thereof.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is, a kind of electric conduction nylon composite material, and it is special
Levy and be, the most composed of the following components:
Electric conduction nylon composite material according to claim 1, it is characterised in that described Graphene is Nanjing pioneer
Carboxylated graphene powder.
Electric conduction nylon composite material according to claim 1, it is characterised in that coupling agent is Nanjing chemical industry forward
KH-550, purity >=97%.
Electric conduction nylon composite material according to claim 1, it is characterised in that described toughener is POE grafting
Maleic anhydride, percent grafting is 0.8%.
Electric conduction nylon composite material according to claim 1, it is characterised in that described antioxidant be N, N'-double-
(3-(3,5-di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, fusing point 110-125 degree Celsius.
The preparation method of electric conduction nylon composite material described in a kind of claim 1, it is characterised in that comprise the following steps:
1) raw material is weighed by above-mentioned percentage by weight；
2) PA1212 is mixed 3-7 minute in a mixer with silicone oil；
3) by step 2) in the PA1212 that mixes exist with silicon oil mixture and coupling agent, toughener, antioxidant, Graphene
Blender mixes 3-7 minute；
4) raw material mixed in step 3) is thrown in double screw extruder, through melt extruding, pelletize.Produce work
Skill condition is: double screw extruder one district temperature is 180-220 DEG C, and two district's temperature are 180-220 DEG C, and three district's temperature are 180-
220 DEG C, four district's temperature are 180-220 DEG C, and compound time of delivery in screw rod is 1-2 minute.
The coupling agent of the present invention can improve Graphene and resin compatible well. and the addition of toughener improves material
Toughness, a small amount of Graphene just can accomplish conduction, the electric conduction nylon composite material conductivity height of the present invention, good toughness, system
Standby process is simple, and production technology is easily controlled.
[detailed description of the invention]
Below by embodiment, the present invention is further elaborated:
A kind of electric conduction nylon composite material that the present invention provides, its composition is by weight percentage:
PA1212 82-90%；Graphene 1-5%；Coupling agent KH-550 0.1-1%；Toughener POE-MAH 8-
13%；Antioxidant 1010 0.1-1%；Silicone oil 0.5-1%；
Wherein, PA1212 is east, Shandong occasion AIVS01.Its impact strength (ASTM D256) is 25KJ/M3.
Antioxidant is the N of Beijing easily chemical industry, N'-is double-(3-(3,5-di-tert-butyl-hydroxy phenyl) propiono) oneself two
Amine 1010, fusing point 110-125 degree Celsius.
Coupling agent is the KH-550 of Nanjing chemical industry forward, and its purity is >=97%.
Toughener is homemade POE grafted maleic anhydride, and percent grafting is 0.8%.The preparation method of POE grafted maleic anhydride
For: each component of following percentage by weight is mixed, extrudes under conditions of temperature is 140-200 DEG C with double screw extruder:
Graphene is the carboxylated graphene powder XF004 of Nanjing pioneer
Silicone oil is common silicone oil.
PA1212 and the silicone coupling agents of Graphene in the present invention, it is possible to improve inorganic and organic compatible very well
Property, and it is little to play addition, but can reach efficient electrical conductivity
Its manufacture process is as follows:
1) raw material is weighed by above-mentioned percentage by weight；
2) PA1212 is mixed 3-7 minute in a mixer with silicone oil；
3) by step 2) in the PA1212 that mixes exist with silicon oil mixture and coupling agent, toughener, antioxidant, Graphene
Blender mixes 3-7 minute；
4) raw material mixed in step 3) is thrown in double screw extruder, through melt extruding, pelletize.Produce work
Skill condition is: double screw extruder one district temperature is 180-220 DEG C, and two district's temperature are 180-220 DEG C, and three district's temperature are 180-
220 DEG C, four district's temperature are 180-220 DEG C, and compound time of delivery in screw rod is 1-2 minute.
Below in conjunction with specific embodiment, the present invention is explained in detail:
Embodiment 1
PA121286.9%；Graphene 1%；Coupling agent KH-5500.5%；Toughener POE-MAH10%；Antioxidant
10100.1%；Silicone oil 0.5%；
First add silicone oil and PA1212 be sufficiently mixed all with, make silicone oil invest PA1212 surface well, add the most again
Graphene powder and other raw material mix so that Graphene can be uniformly dispersed in resin.
It is 200-260 DEG C of double screw extruder extrusion through melt temperature, pelletize.
The most each zone temperatures is: 180 DEG C of a district, two 200 DEG C of districts, three 220 DEG C of districts, four 220 DEG C of districts, and five 220 DEG C of districts stop
Staying the time is 90 seconds.
Embodiment 2
PA121284.9%；Graphene 2%；Coupling agent KH-5500.5%；Toughener POE-MAH10%；Antioxidant
10100.1%；Silicone oil 0.5%；
First add silicone oil and PA1212 be sufficiently mixed all with, make silicone oil invest PA1212 surface well, add the most again
Graphene powder and other raw material mix so that Graphene can be uniformly dispersed in resin.
It is 200-260 DEG C of double screw extruder extrusion through melt temperature, pelletize.
The most each zone temperatures is: 180 DEG C of a district, two 200 DEG C of districts, three 220 DEG C of districts, four 220 DEG C of districts, and five 220 DEG C of districts stop
Staying the time is 90 seconds.
Embodiment 3
PA121282.9%；Graphene 3%；Coupling agent KH-5500.5%；Toughener POE-MAH10%；Antioxidant 1010
0.1%；Silicone oil 0.5%；
First add silicone oil and PA1212 be sufficiently mixed all with, make silicone oil invest PA1212 surface well, add the most again
Graphene powder and other raw material mix so that Graphene can be uniformly dispersed in resin.
It is 200-260 DEG C of double screw extruder extrusion through melt temperature, pelletize.
The most each zone temperatures is: 180 DEG C of a district, two 200 DEG C of districts, three 220 DEG C of districts, four 220 DEG C of districts, and five 220 DEG C of districts stop
Staying the time is 90 seconds.
Embodiment 4
PA121280.9%；Graphene 4%；Coupling agent KH-5500.5%；Toughener POE-MAH10%；Antioxidant
10100.1%；Silicone oil 0.5%；
First add silicone oil and PA1212 be sufficiently mixed all with, make silicone oil invest PA1212 surface well, add the most again
Graphene powder and other raw material mix so that Graphene can be uniformly dispersed in resin.
It is 200-260 DEG C of double screw extruder extrusion through melt temperature, pelletize.
The most each zone temperatures is: 180 DEG C of a district, two 200 DEG C of districts, three 220 DEG C of districts, four 220 DEG C of districts, and five 220 DEG C of districts stop
Staying the time is 90 seconds.
Embodiment 5
PA121283.9%；Graphene 1%；Coupling agent KH-5501%；Toughener POE-MAH13%；Antioxidant 1010 0.1%；
Silicone oil 1%；
First add silicone oil and PA1212 be sufficiently mixed all with, make silicone oil invest PA1212 surface well, add the most again
Graphene powder and other raw material mix so that Graphene can be uniformly dispersed in resin.
It is 200-260 DEG C of double screw extruder extrusion through melt temperature, pelletize.
The most each zone temperatures is: 180 DEG C of a district, two 200 DEG C of districts, three 220 DEG C of districts, four 220 DEG C of districts, and five 220 DEG C of districts stop
Staying the time is 90 seconds.
Performance test:
Above-mentioned 5 embodiments complete the particle of pelletize be dried 4-6 hour in the convection oven of 80-100 DEG C, then will be dry
Dry particle is molded sample preparation on 80T injection machine, keeps mould temperature in sample making course between 70-100 DEG C.
Hot strength is tested by GB/T1040 standard, and specimen types is I type, batten size (mm): 170(length) ×
(20 ± 0.2) (end portion width) × (4 ± 0.2) (thickness), draw speed is 50mm/min；
Bending strength and bending modulus are tested by GB9341/T standard.Specimen types is specimen size (mm): (80 ±
2) × (10 ± 0.2) × (4 ± 0.2), rate of bending is 20mm/min；
Notch impact strength is tested by GB/T1043 standard, and specimen types is I type, specimen size (mm): (80 ± 2)
× (10 ± 0.2) × (4 ± 0.2)；Breach type is A class, and breach residual thickness is 3.2mm；
Plastic cement antistatic (electrical conductivity) test is tested by GB/T15662-1995 standard.Table 1: embodiment 1-5
Formula table
| Component (percentage by weight) | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| PA1212 | 87.9 | 86.9 | 85.9 | 84.9 | 83.9 |
| Graphene | 1 | 2 | 3 | 4 | 1 |
| Toughener | 10 | 10 | 10 | 10 | 13 |
| Coupling agent | 0.5 | 0.5 | 0.5 | 0.5 | 1 |
| Antioxidant | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Silicone oil | 0.5 | 0.5 | 0.5 | 0.5 | 1 |
Table 2: being shown in Table of embodiment 1-5
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Notch impact strength (J/M) | 600 | 625 | 665 | 668 | 690 |
| Hot strength (MPa) | 36 | 35 | 40 | 43 | 42 |
| Bending strength (MPa) | 45 | 43 | 48 | 47 | 46 |
| Electrical conductivity (Ω m) | 106 | 104 | 103 | 102 | 102 |
| Bending modulus (MPa) | 1320 | 1600 | 1585 | 880 | 1450 |
It is the hardest nano material also that Graphene is currently the thinnest, and it is almost fully transparent, only absorbs
The light of 2.3%；Heat conductivity is up to 5300W/m K, and higher than CNT and diamond, under room temperature, its electron mobility * exceedes
15000cm²/ V s higher than CNT or silicon crystal * again, and resistivity only about 10-6 Ω cm, than copper or silver more more
Low, for the material that resistivity in the world is minimum
By learning after the data analysis in above table, the overall performance to composite that adds of Graphene has one
Fixed lifting effect, particularly impact strength, the nanostructured of the main still Graphene true qualities of reason, thus entirety is combined
The material property effect of haveing a certain upgrade, from the point of view of electrical conductivity, Graphene typically add 1% reached one anti-quiet
Electricity effect, for electrically conductive graphite, has greatly reduced adding proportion, along with the increase of Graphene adding proportion, has led
Electrostrictive coefficient also promotes, when adding proportion more than or equal to 2% when, integral material the most can reach conductive effect, therefore,
Graphene is filled PA1212 and the performance of material is not only had castering action, and also gives good conductive effect.
The coupling agent of the siloxanes in above example of the present invention can improve Graphene and resin compatible well. stone
Before ink alkene adds, first add a certain amount of silicone oil and resin be sufficiently mixed all with, accomplish that silicone oil can be good at investing resin
Surface, adds Graphene powder the most again so that Graphene can be uniformly dispersed in resin.The addition of self-control toughener is direct
Improve the toughness of material.The impact of the original material of PA1212 is the most superior, and water absorption rate is low, to some dimensional requirements
High product also is adapted for, as long as adding a small amount of Graphene just can accomplish conduction, owing to Graphene belongs to Nano grade, because of
The performance of material is not only reduced after adding by this, can be improved on the contrary in terms of impact strength.
The composite conducting material its preparation method that a kind of Graphene provided by the present invention is filled PA1212 above is carried out
Being discussed in detail, principle and the embodiment of the present invention are set forth by specific case used herein, above example
Explanation be only intended to help to understand method and the core concept thereof of the present invention；Simultaneously for one of ordinary skill in the art,
According to the thought of the present invention, the most all will change, to sum up, this specification content is not
It is interpreted as limitation of the present invention.
Claims (5)
1. an electric conduction nylon composite material, it is characterised in that the most composed of the following components:
Each component sum is 100%；Toughener is POE grafted maleic anhydride, and percent grafting is 0.8%；POE grafted maleic anhydride
Preparation method is: each component of following percentage by weight mixed, and is the condition of 140-200 DEG C with double screw extruder in temperature
Lower extrusion:
Electric conduction nylon composite material the most according to claim 1, it is characterised in that described Graphene is Nanjing pioneer's
Carboxylated graphene powder.
Electric conduction nylon composite material the most according to claim 1, it is characterised in that coupling agent is Nanjing chemical industry forward
KH-550, purity >=97%.
Electric conduction nylon composite material the most according to claim 1, it is characterised in that described antioxidant be N, N'-double-
(3-(3,5-di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, fusing point 110-125 degree Celsius.
5. the preparation method of electric conduction nylon composite material described in a claim 1, it is characterised in that comprise the following steps:
1) percentage by weight as described in claim 1 weighs raw material；
2) PA1212 is mixed 3-7 minute in a mixer with silicone oil；
3) by step 2) in the PA1212 that mixes mixing with coupling agent, toughener, antioxidant, Graphene with silicon oil mixture
Device mixes 3-7 minute；
4) by step 3) in the raw material that mixes throw in double screw extruder, through melt extruding, pelletize；Production technology bar
Part is: double screw extruder one district temperature is 180-220 DEG C, and two district's temperature are 180-220 DEG C, and three district's temperature are 180-220 DEG C,
Four district's temperature are 180-220 DEG C, and compound time of delivery in screw rod is 1-2 minute.
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| CN201310745328.1A CN103740102B (en) | 2013-12-27 | 2013-12-27 | A kind of electric conduction nylon composite material and preparation method thereof |
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| CN201310745328.1A CN103740102B (en) | 2013-12-27 | 2013-12-27 | A kind of electric conduction nylon composite material and preparation method thereof |
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| CN104086983B (en) * | 2014-07-28 | 2016-09-28 | 北京中科博益科技有限公司 | Graphene/nylon composite materials and its preparation method and application |
| CN107227019B (en) * | 2017-04-27 | 2019-09-20 | 宁波海雨新材料科技有限公司 | A kind of 66 composite material and preparation method of graphene conductive modification of nylon |
| CN108863312A (en) * | 2018-07-12 | 2018-11-23 | 李磊 | A kind of Antistatic ceramic high performance antistatic agent and preparation method thereof |
| CN111518388B (en) * | 2020-05-21 | 2023-04-25 | 长沙五犇新材料科技有限公司 | High-strength high-temperature-resistant conductive nylon composite material and preparation method thereof |
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| CN103044906A (en) * | 2012-12-31 | 2013-04-17 | 广东高怡新工程塑料有限公司 | Nylon base composite material with heat conducting function, and preparation method of nylon base composite material |
| CN103384696A (en) * | 2010-12-21 | 2013-11-06 | 巴斯夫欧洲公司 | Thermoplastic molding composition |
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| CN103384696A (en) * | 2010-12-21 | 2013-11-06 | 巴斯夫欧洲公司 | Thermoplastic molding composition |
| CN103044906A (en) * | 2012-12-31 | 2013-04-17 | 广东高怡新工程塑料有限公司 | Nylon base composite material with heat conducting function, and preparation method of nylon base composite material |
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