CN103102683B - Preparation method of carbon nanotube/polyamide 66 composite material - Google Patents
Preparation method of carbon nanotube/polyamide 66 composite material Download PDFInfo
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- CN103102683B CN103102683B CN201310051533.8A CN201310051533A CN103102683B CN 103102683 B CN103102683 B CN 103102683B CN 201310051533 A CN201310051533 A CN 201310051533A CN 103102683 B CN103102683 B CN 103102683B
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Abstract
The invention relates to a preparation method of a carbon nanotube/polyamide 66 composite material, which comprises the following steps: performing oxidation, acylating chlorination and amination on the carbon nanotube, performing melt blending to synthetize the carbon nanotube/polyamide 66 composite material, extruding for granulation, performing melt mixing, and uniformly dispersing the carbon nanotube in a polyamide 66 matrix. the strength, high temperature resistance, antioxidation, corrosion resistance performances of polyamide 66 can be effectively enhanced, the frictional coefficient of the composite material can be reduced, the preparation method has advanced and reasonable technology, the data is definite and accurate, the product has good quality, the prepared polyamide 66 can be used in a plurality of industrial fields, and is an ideal enhancement preparation method of the polyamide 66 composite material.
Description
Technical field
The present invention relates to a kind of preparation method of carbon nano tube/polyamide 6 amine 66 matrix material, belong to the technical field of the preparations and applicatio of carbon material/polymer composites.
Background technology
Polymer matrix composite is a kind of desirable friction materials, polyamide 66 is one of material the most frequently used in plastics, polyamide 66 has high physical strength, its softening temperature is high, heat-resisting, coefficient of friction is low, wear-resistant, self lubricity, shock absorption, sound-deadening properties, oil-proofness, weak acid resistant, alkali resistance, electrical insulating property are good, has self-extinguishing, nontoxic, odorless feature; And also can keep higher strength and stiffness at comparatively high temps, be applicable to the application of motor car engine and periphery heat-resistant part, but also there is resistance to strong acid, strong basicity is poor, water-intake rate is large shortcoming in polyamide 66, thus affects the stability of its product size, limits its range of application.
For the defect of the chemical physics performance of polyamide 66, the normal method adopting other chemical substances of doping, but still there is the problem of unstable properties, the material selected had is unreasonable, technical parameter is inaccurate, preparation method's imprecision, does not still reach the performance requriements of polyamide 66.
Summary of the invention
Goal of the invention
The object of the invention is the practical situation for background technology, carbon nanotube is adopted to be polymerized with polyamide 66 melt blending, by oxide treatment, modifying and decorating, the melt polymerization of carbon nanotube, carbon nanotube and polyamide 66 are mixed and made into matrix material, to increase substantially the chemical physics performance of polyamide 66, strengthen acidproof, alkali resistance and water-retaining capacity, expand the range of application of polyamide 66.
Technical scheme
The chemical substance material that the present invention uses is: carbon nanotube, polyamide 66, sulfuric acid, nitric acid, sulfur oxychloride, N, dinethylformamide, quadrol, tetrahydrofuran (THF), dehydrated alcohol, deionized water, it is as follows that its combination prepares consumption: with gram, milliliter for measure unit
Carbon nanotube: C 10g ± 0.001g
Polyamide 66: [NH (CH
2)
6-NHCO (CH
2)
4cO]
nn=200 100g ± 0.001g
Sulfuric acid: H
2sO
4200mL ± 1mL
Nitric acid: HNO
3100mL ± 1mL
DMF: HCON (CH
3)
220mL ± 1mL
Sulfur oxychloride: SOCl
2100mL ± 1mL
Quadrol: NH
2(CH
2)
2nH
2300mL ± 1mL
Tetrahydrofuran (THF): C
4h
8o 500mL ± 1mL
Dehydrated alcohol: C
2h
5oH 1000mL ± 10mL
Deionized water: H
2o 20000mL ± 100mL
Preparation method is as follows:
(1) selected chemical substance material
To carry out selected to the chemical substance material that preparation uses, and carry out quality purity, concentration control:
Carbon nanotube: solid state diameter≤Φ 50 nm, length≤20 μm, purity > 99 %
Polyamide 66: solid state, 99%
Sulfuric acid: liquid liquid concentration 98%
Nitric acid: liquid liquid concentration 65%
DMF: liquid liquid 99.5%
Sulfur oxychloride: liquid liquid 99.5%
Quadrol: liquid liquid 99%
Tetrahydrofuran (THF): liquid liquid 99%
Dehydrated alcohol: liquid liquid 99.7%
Deionized water: liquid liquid 99.99%
(2) grind, sieve, thinning processing carbon nanotube
Carbon nanotube agate mortar, pestle ground, then sieves with 650 eye mesh screens, grind, sieve and repeatedly carry out;
(3) oxide treatment carbon nanotube
Oxide treatment carbon nanotube carries out on there-necked flask, ultrasonic disperse instrument, completes under ultrasonic water heating, stirring;
1. take carbon nanotube 3g ± 0.001g, add in there-necked flask, be then placed on ultrasonic disperse instrument;
2. open ultrasonic disperse instrument, under ultrasonic frequency 50kHz, Heating temperature 50 DEG C ± 2 DEG C, adds sulfuric acid 180mL, nitric acid 60mL;
3. the stirring magneton in there-necked flask starts to stir, and churning time 120min ± 2min becomes: oxide solution;
4. carbon nanotube will carry out chemical reaction in oxidation reaction process, and reaction formula is as follows:
In formula:
C-COOH: carboxylic oxide/carbon nanometer tube
SO
2: sulfurous gas
NO
2: nitrogen peroxide
CO
2: carbonic acid gas
5., after oxidizing reaction, close ultrasonic disperse instrument, make the oxide solution in there-necked flask be cooled to 25 DEG C;
6. suction filtration, is placed in the Büchner funnel of filter flask by oxide solution, carry out suction filtration with millipore filtration, remaining product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. deionized water wash, suction filtration
Product cake is placed in beaker, adds deionized water 1000mL, agitator treating 5min;
Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Deionized water wash, suction filtration repeat five times;
8. vacuum-drying, is placed in vacuum drying oven by product cake and carries out drying, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, and time of drying 8, h, obtained after drying: carboxylic oxide/carbon nanometer tube;
(4) chloride of carbon nanotube
The chloride of carbon nanotube is carried out on there-necked flask, oil bath cylinder, electric heating agitator;
1. carboxylic oxide/carbon nanometer tube 3 g ± 0.001g is added in there-necked flask;
DMF 5 mL is added in there-necked flask;
Sulfur oxychloride 100 mL is added in there-necked flask;
2. open electric heating agitator, Heating temperature 70 DEG C ± 2 DEG C, and stir;
3. heat, stir 24 h, carry out modification reaction;
4. chemical reaction will occur in the reaction of chloride modification, reaction formula is as follows:
In formula:
C-COCl: chloride carbon nanotube
SO
2: sulfurous gas
5. after modification, modified-reaction, close electric heating agitator, stop heated and stirred, make it be cooled to 25 DEG C with bottle: modification solution;
6. suction filtration, is placed in the Büchner funnel of filter flask by modification solution, carry out suction filtration with millipore filtration, remaining product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. tetrahydrofuran (THF) washing, suction filtration
Product cake is placed in beaker, adds tetrahydrofuran (THF) 200mL, agitator treating 5min;
Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Tetrahydrofuran (THF) washing, suction filtration are clarified to filtrate;
8. vacuum-drying, is placed in vacuum drying oven by product cake and carries out drying, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, and time of drying 8, h, obtained after drying: chloride carbon nanotube;
(5) carbon nanotube is aminated
The aminated of carbon nanotube carries out on there-necked flask, oil bath cylinder, electric heating agitator,
1. chloride carbon nanotube 1.5 g ± 0.001g is added in there-necked flask;
Quadrol 300 mL is added in there-necked flask;
2. open electric heating agitator, oil bath cylinder Heating temperature 100 DEG C ± 2 DEG C, and stir;
3. constant temperature stirs 48 h, carries out aminated reaction; ,
4. chemical reaction will occur in aminated reaction, reaction formula is as follows:
In formula:
C-CONH (CH
2)
2nH
2: aminated carbon nanotube
HCl: hydrogenchloride
5. after reaction, close electric heating agitator, stop stirring, make it be cooled to 25 DEG C with bottle: aminated solution;
6. suction filtration, is placed in the Büchner funnel of filter flask by aminated solution, carry out suction filtration with millipore filtration, remaining product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. absolute ethanol washing, suction filtration
Product cake is placed in beaker, adds dehydrated alcohol 200mL, agitator treating 5min;
Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Absolute ethanol washing, suction filtration repeat five times;
8. vacuum-drying, is placed in vacuum drying oven by product cake and carries out drying, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, and time of drying 8, h, obtained after drying: the carbon nanotube of aminated modification;
(6) carbon nano tube/polyamide 6 amine 66 matrix material is prepared
1. vacuum-drying, by polyamide 66,60g ± 0.001g, carries out vacuum dehydration in vacuum drying oven, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, time of drying 12 h;
2. extruding pelletization
By polyamide 66,60g ± 0.0001g, aminated carbon nanotube 1.5g ± 0.001g, joins in compounding extruder, mixes;
Forcing machine Heating temperature is 260 DEG C ± 5 DEG C, squeeze pressure 45MPa, extruding 5s interval time, polyamide 66, aminated carbon nanotube mixture are added in twin screw extruder, extrudate, through cooling trough cooling, dicing machine cutting, becomes particulate state, particle diameter≤Φ 1mm, length≤5mm;
After extruding be: carbon nano tube/polyamide 6 amine 66 matrix material;
(7) vacuum-drying, dehydration
Carbon nano tube/polyamide 6 amine 66 particle is carried out drying and dehydrating in vacuum drying oven, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, time of drying 12 h;
(8) detect, analyze, characterize
The pattern of carbon nano tube/polyamide 6 amine 66 matrix material of preparation, structure, composition, chemical physics performance, frictional behaviour are detected, analyze, characterized;
Morphology analysis is carried out with field emission scanning electron microscope;
Surface functional group analysis is carried out with infrared spectrometer;
Crystal structure analysis is carried out with X-ray diffractometer;
Thermal stability analysis is carried out with thermogravimetric analyzer;
Crystallinity analysis is carried out by differential scanning calorimeter;
Mechanics property analysis is carried out with universal tensile instrument;
Micro Mechanical Properties analysis is carried out with nano-hardness tester;
Analysis on Friction Performance is carried out with frictional testing machines;
Conclusion: carbon nano tube/polyamide 6 amine 66 matrix material is dark circles cylindrical particle, particle diameter≤Φ 1mm, length≤5mm, smooth surface, the frictional coefficient of its matrix material reduces by 0.1;
(9) product storage
Be stored in amber transparent Glass Containers to carbon nano tube/polyamide 6 amine 66 matrix material of preparation, airtightly keep in Dark Place, waterproof, sun-proof, moistureproof, anti-acid-alkali salt to corrode, storing temp 20 DEG C ± 2 DEG C, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, have employed brand-new preparation technology's flow process, first carbon nanotube is oxidized, chloride, aminated process, by melt blending synthesizing carbon nanotubes/polyamide 66 composite material, through extruding pelletization melting mixing, even carbon nanotube is made to be dispersed in polyamide 66 matrix, obtain finely dispersed matrix material, improve the intensity of polyamide 66, high temperature resistant, anti-oxidant, erosion resistance, and the frictional coefficient of matrix material can be reduced, this preparation method's technique is tight, rationally advanced, informative data is accurate, product quality is good, the polyamide 66 of preparation can be applied at multiple industrial circle, the enhancing preparation method of very good polyamide 66 composite material.
Accompanying drawing explanation
Fig. 1 is the state graph of carbon nano tube/polyamide 6 amine 66 extruding pelletization
Fig. 2 is that carbon nano tube/polyamide 6 amine 66 matrix material amplifies 10000 times of scanning shape appearance figures
Fig. 3 is carbon nano tube/polyamide 6 amine 66 composite materials property graphic representation
Fig. 4 is that 10000 scanning shape appearance figures are amplified in carbon nano tube/polyamide 6 amine 66 matrix material tension fracture face
Fig. 5 is the frictional behaviour graphic representation of carbon nano tube/polyamide 6 amine 66 matrix material
Shown in figure, list of numerals is as follows:
1. extrude support, 2. extrude motor, 3. feed sleeve, 4. extrusion screw sleeve; 5. cooling tank, 6. cooling trough, 7. air dryer, 8. dicing machine; 9. discharge port, 10. product case, 11. carbon nanotube hoppers, 12. polyamide 66 hoppers; 13. well heaters, 14. electric control boxs, 15. display screens; 16. pilot lamp, 17. extruding motor modulators, 18. air dryer modulators; 19. dicing machine modulators, 20. well heater modulators, 21. wires.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, be the state graph of carbon nano tube/polyamide 6 amine 66 extruder grain, each position, annexation will correctly, according to quantity proportioning, operate according to the order of sequence.
The value of the chemical substance that preparation uses determines by the scope pre-set, with gram, milliliter for measure unit.
The extruder grain of carbon nano tube/polyamide 6 amine 66 matrix material is shaping to carry out on extrusion machine, completes in batch mixing, heating, extrusion screw extruding, cooling, air-dry, pelletizing process;
Extrusion machine is horizontal, extruding the left part of support 1 for extruding motor 2, feed sleeve 3 on the right part connection extruder seat 1 of extruding motor 2, feed sleeve 3 right part connects extrusion screw sleeve 4, extrusion screw sleeve 4 right part connects cooling tank 5 and cooling trough 6, and cooling tank 5 right part connects air dryer 7, and air dryer 7 right part connects dicing machine 8, dicing machine 8 right part is discharge port 9, and discharge port 9 aims at product case 10; Carbon nanotube hopper 11, polyamide 66 hopper 12 are set on the top of feed sleeve 3; Be well heater 13 in the bottom of extrusion screw sleeve 4; Extruding motor 2 left part be electric control box 14; electric control box 14 arranges display screen 15, pilot lamp 16, extruding motor modulator 17, air dryer modulator 18, dicing machine modulator 19, and electric control box 14 is connected with extruding motor 2, well heater 13, air dryer 7, dicing machine 8 by wire 21.
Shown in Fig. 2, be carbon nano tube/polyamide 6 amine 66 matrix material shape appearance figure, known in figure: white bright spot is carbon nanotube, evenly divide in polyamide 66 matrix, ruler units 1 μm.
Shown in Fig. 3, for carbon nano tube/polyamide 6 amine 66 composite materials property graphic representation, ordinate zou is stress intensity, X-coordinate is strain value, a curve is the stress-strain(ed) curve of polyamide 66, b curve is the stress-strain(ed) curve of carbon nano tube/polyamide 6 amine 66 matrix material, the tensile strength of matrix material b improves 12.7%, and modulus improves 24.2%, and the mechanical property of matrix material significantly improves.
Shown in Fig. 4, for 10000 times of scanning shape appearance figures are amplified in amination carbon nano tube/polyamide 6 amine 66 matrix material tension fracture face, known in figure: amination even carbon nanotube is dispersed in polyamide 66 matrix, and carbon nanotube is drawn out from polyamide 66 matrix at surface of fracture place, ruler units 1 μm.
Shown in Fig. 5, for the frictional behaviour graphic representation of carbon nano tube/polyamide 6 amine 66 matrix material, ordinate zou is frictional coefficient, X-coordinate is wearing-in period, c curve is the friction coefficient curve of polyamide 66, d curve is the friction coefficient curve of carbon nano tube/polyamide 6 amine 66 matrix material, the average friction coefficient of matrix material d reduces 0.1, and the frictional behaviour of matrix material significantly improves.
Claims (2)
1. the preparation method of carbon nano tube/polyamide 6 amine 66 matrix material, it is characterized in that: the chemical substance material of use is: carbon nanotube, polyamide 66, sulfuric acid, nitric acid, sulfur oxychloride, N, dinethylformamide, quadrol, tetrahydrofuran (THF), dehydrated alcohol, deionized water, it is as follows that its combination prepares consumption: with gram, milliliter for measure unit
Carbon nanotube: C 10g ± 0.001g
Polyamide 66: [NH (CH
2)
6-NHCO (CH
2)
4cO]
nn=200 100g ± 0.001g
Sulfuric acid: H
2sO
4200mL ± 1mL
Nitric acid: HNO
3100mL ± 1mL
DMF: HCON (CH
3)
220mL ± 1mL
Sulfur oxychloride: SOCl
2100mL ± 1mL
Quadrol: NH
2(CH
2)
2nH
2300mL ± 1mL
Tetrahydrofuran (THF): C
4h
8o 500mL ± 1mL
Dehydrated alcohol: C
2h
5oH 1000mL ± 10mL
Deionized water: H
2o 20000mL ± 100mL
Preparation method is as follows:
(1) selected chemical substance material
To carry out selected to the chemical substance material that preparation uses, and carry out quality purity, concentration control:
Carbon nanotube: solid state diameter≤Φ 50 nm, length≤20 μm, purity > 99 %
Polyamide 66: solid state, 99%
Sulfuric acid: liquid liquid concentration 98%
Nitric acid: liquid liquid concentration 65%
DMF: liquid liquid 99.5%
Sulfur oxychloride: liquid liquid 99.5%
Quadrol: liquid liquid 99%
Tetrahydrofuran (THF): liquid liquid 99%
Dehydrated alcohol: liquid liquid 99.7%
Deionized water: liquid liquid 99.99%
(2) grind, sieve, thinning processing carbon nanotube
Carbon nanotube agate mortar, pestle ground, then sieves with 650 eye mesh screens, grind, sieve and repeatedly carry out;
(3) oxide treatment carbon nanotube
Oxide treatment carbon nanotube carries out on there-necked flask, ultrasonic disperse instrument, completes under ultrasonic water heating, stirring;
1. take carbon nanotube 3g ± 0.001g, add in there-necked flask, be then placed on ultrasonic disperse instrument;
2. open ultrasonic disperse instrument, under ultrasonic frequency 50kHz, Heating temperature 50 DEG C ± 2 DEG C, adds sulfuric acid 180mL, nitric acid 60mL;
3. the stirring magneton in there-necked flask starts to stir, and churning time 120min ± 2min becomes: oxide solution;
4. carbon nanotube will carry out chemical reaction in oxidation reaction process, and reaction formula is as follows:
In formula:
C-COOH: carboxylic oxide/carbon nanometer tube
SO
2: sulfurous gas
NO
2: nitrogen peroxide
CO
2: carbonic acid gas
5., after oxidizing reaction, close ultrasonic disperse instrument, make the oxide solution in there-necked flask be cooled to 25 DEG C;
6. suction filtration, is placed in the Büchner funnel of filter flask by oxide solution, carry out suction filtration with millipore filtration, remaining product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. deionized water wash, suction filtration
Product cake is placed in beaker, adds deionized water 1000mL, agitator treating 5min;
Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Deionized water wash, suction filtration repeat five times;
8. vacuum-drying, is placed in vacuum drying oven by product cake and carries out drying, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, and time of drying 8, h, obtained after drying: carboxylic oxide/carbon nanometer tube;
(4) chloride of carbon nanotube
The chloride of carbon nanotube is carried out on there-necked flask, oil bath cylinder, electric heating agitator;
1. carboxylic oxide/carbon nanometer tube 3 g ± 0.001g is added in there-necked flask;
DMF 5 mL is added in there-necked flask;
Sulfur oxychloride 100 mL is added in there-necked flask;
2. open electric heating agitator, Heating temperature 70 DEG C ± 2 DEG C, and stir;
3. heat, stir 24 h, carry out modification reaction;
4. chemical reaction will occur in the reaction of chloride modification, reaction formula is as follows:
In formula:
C-COCl: chloride carbon nanotube
SO
2: sulfurous gas
5. after modification, modified-reaction, close electric heating agitator, stop heated and stirred, make it be cooled to 25 DEG C with bottle: modification solution;
6. suction filtration, is placed in the Büchner funnel of filter flask by modification solution, carry out suction filtration with millipore filtration, remaining product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. tetrahydrofuran (THF) washing, suction filtration
Product cake is placed in beaker, adds tetrahydrofuran (THF) 200mL, agitator treating 5min;
Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Tetrahydrofuran (THF) washing, suction filtration are clarified to filtrate;
8. vacuum-drying, is placed in vacuum drying oven by product cake and carries out drying, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, and time of drying 8, h, obtained after drying: chloride carbon nanotube;
(5) carbon nanotube is aminated
The aminated of carbon nanotube carries out on there-necked flask, oil bath cylinder, electric heating agitator,
1. chloride carbon nanotube 1.5 g ± 0.001g is added in there-necked flask;
Quadrol 300 mL is added in there-necked flask;
2. open electric heating agitator, oil bath cylinder Heating temperature 100 DEG C ± 2 DEG C, and stir;
3. constant temperature stirs 48 h, carries out aminated reaction; ,
4. chemical reaction will occur in aminated reaction, reaction formula is as follows:
In formula:
C-CONH (CH
2)
2nH
2: aminated carbon nanotube
HCl: hydrogenchloride
5. after reaction, close electric heating agitator, stop stirring, make it be cooled to 25 DEG C with bottle: aminated solution;
6. suction filtration, is placed in the Büchner funnel of filter flask by aminated solution, carry out suction filtration with millipore filtration, remaining product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. absolute ethanol washing, suction filtration
Product cake is placed in beaker, adds dehydrated alcohol 200mL, agitator treating 5min;
Then washings is placed in the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, remaining product filter cake on filter membrane, washings is evacuated in filter flask;
Absolute ethanol washing, suction filtration repeat five times;
8. vacuum-drying, is placed in vacuum drying oven by product cake and carries out drying, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, and time of drying 8, h, obtained after drying: the carbon nanotube of aminated modification;
(6) carbon nano tube/polyamide 6 amine 66 matrix material is prepared
1. vacuum-drying, by polyamide 66,60g ± 0.001g, carries out vacuum dehydration in vacuum drying oven, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, time of drying 12 h;
2. extruding pelletization
By polyamide 66,60g ± 0.0001g, aminated carbon nanotube 1.5g ± 0.001g, joins in compounding extruder, mixes;
Forcing machine Heating temperature is 260 DEG C ± 5 DEG C, squeeze pressure 45MPa, extruding 5s interval time, polyamide 66, aminated carbon nanotube mixture are added in twin screw extruder, extrudate, through cooling trough cooling, dicing machine cutting, becomes particulate state, particle diameter≤Φ 1mm, length≤5mm;
After extruding be: carbon nano tube/polyamide 6 amine 66 matrix material;
(7) vacuum-drying, dehydration
Carbon nano tube/polyamide 6 amine 66 particle is carried out drying and dehydrating in vacuum drying oven, drying temperature 80 DEG C ± 2 DEG C, vacuum tightness 10Pa, time of drying 12 h;
(8) detect, analyze, characterize
The pattern of carbon nano tube/polyamide 6 amine 66 matrix material of preparation, structure, composition, chemical physics performance, frictional behaviour are detected, analyze, characterized;
Morphology analysis is carried out with field emission scanning electron microscope;
Surface functional group analysis is carried out with infrared spectrometer;
Crystal structure analysis is carried out with X-ray diffractometer;
Thermal stability analysis is carried out with thermogravimetric analyzer;
Crystallinity analysis is carried out by differential scanning calorimeter;
Mechanics property analysis is carried out with universal tensile instrument;
Micro Mechanical Properties analysis is carried out with nano-hardness tester;
Analysis on Friction Performance is carried out with frictional testing machines;
Conclusion: carbon nano tube/polyamide 6 amine 66 matrix material is dark circles cylindrical particle, particle diameter≤Φ 1mm, length≤5mm, smooth surface, the frictional coefficient of its matrix material reduces by 0.1;
(9) product storage
Be stored in amber transparent Glass Containers to carbon nano tube/polyamide 6 amine 66 matrix material of preparation, airtightly keep in Dark Place, waterproof, sun-proof, moistureproof, anti-acid-alkali salt to corrode, storing temp 20 DEG C ± 2 DEG C, relative humidity≤10%.
2. the preparation method of a kind of carbon nano tube/polyamide 6 amine 66 matrix material according to claim 1, it is characterized in that: the extruder grain of carbon nano tube/polyamide 6 amine 66 matrix material is shaping to carry out on extrusion machine, complete in batch mixing, heating, extrusion screw extruding, cooling, air-dry, pelletizing process;
Extrusion machine is horizontal, extruding the left part of support (1) for extruding motor (2), feed sleeve (3) on the right part connection extruder seat (1) of extruding motor (2), feed sleeve (3) right part connects extrusion screw sleeve (4), extrusion screw sleeve (4) right part connects cooling tank (5) and cooling trough (6), cooling tank (5) right part connects air dryer (7), air dryer (7) right part connects dicing machine (8), dicing machine (8) right part is discharge port (9), discharge port (9) aims at product case (10), carbon nanotube hopper (11), polyamide 66 hopper (12) are set on the top of feed sleeve (3), be well heater (13) in the bottom of extrusion screw sleeve (4), extruding motor (2) left part be electric control box (14), electric control box (14) arranges display screen (15), pilot lamp (16), extruding motor modulator (17), air dryer modulator (18), dicing machine modulator (19), and electric control box (14) is connected with extruding motor (2), well heater (13), air dryer (7), dicing machine (8) by wire (21).
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| CN101085863A (en) * | 2007-07-05 | 2007-12-12 | 上海扬泽纳米新材料有限公司 | Conducing composite material and preparation method thereof |
| CN101195709A (en) * | 2007-12-06 | 2008-06-11 | 同济大学 | Method for producing high decentrality amido carbon nano-tube/nylon 66 composite material |
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| CN101085863A (en) * | 2007-07-05 | 2007-12-12 | 上海扬泽纳米新材料有限公司 | Conducing composite material and preparation method thereof |
| CN101195709A (en) * | 2007-12-06 | 2008-06-11 | 同济大学 | Method for producing high decentrality amido carbon nano-tube/nylon 66 composite material |
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| 彭治汉等.塑料工业手册—聚酰胺.《塑料工业手册—聚酰胺》.化学工业出版社,2001,(第1版), * |
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