CN103102683A - 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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- CN103102683A CN103102683A CN2013100515338A CN201310051533A CN103102683A CN 103102683 A CN103102683 A CN 103102683A CN 2013100515338 A CN2013100515338 A CN 2013100515338A CN 201310051533 A CN201310051533 A CN 201310051533A CN 103102683 A CN103102683 A CN 103102683A
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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 carbon nano tube/polyamide 6 amine 66 composite manufacture methods, belong to the preparation of carbon material/polymer composites and the technical field of application.
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, noise reduction, oil-proofness, weak acid resistant, alkali resistance, electrical insulating property are good, and self-extinguishing, nontoxic, odorless characteristics are arranged; And also can keep higher strength and stiffness at comparatively high temps, be fit to the application of motor car engine and peripheral heat-resistant part, but polyamide 66 also exists anti-strong acid, strong basicity is poor, water-intake rate is large shortcoming, thereby affects the stability of its product size, has limited its range of application.
For the defective of the chemical physics performance of polyamide 66, the normal method that adopts other chemical substances of doping, but still have the unsettled problem of performance, the material of selecting that has is unreasonable, technical parameter is inaccurate, and preparation method's imprecision does not still reach the performance requriements of polyamide 66.
Summary of the invention
Goal of the invention
The objective of the invention is the practical situation for background technology, adopt carbon nanotube and polyamide 66 melt blending to carry out polymerization, oxide treatment, modifying and decorating, melt polymerization by 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, enlarge 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 consumption is prepared in its combination: take gram, milliliter as 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
The preparation method is as follows:
(1) selected chemical substance material
The chemical substance material that preparation is used will carry out selected, and carry out quality purity, concentration is controlled:
Carbon nanotube: solid-state solid diameter≤Φ 50 nm, length≤20 μ m, purity＞99 %
Polyamide 66: solid-state solid, 99%
Sulfuric acid: liquid strength of fluid 98%
Nitric acid: liquid strength of fluid 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, the thinning processing carbon nanotube
Carbon nanotube is ground with agate mortar, pestle, then sieve with 650 eye mesh screens, grind, sieve and repeatedly carry out;
(3) oxide treatment carbon nanotube
The oxide treatment carbon nanotube carries out on there-necked flask, ultra-sonic dispersion instrument, completes under ultrasonic water heating, stirring;
1. take carbon nanotube 3g ± 0.001g, add in there-necked flask, then be placed on the ultra-sonic dispersion instrument;
2. open the ultra-sonic dispersion instrument, under ultrasonic frequency 50kHz, 50 ℃ ± 2 ℃ of Heating temperatures add sulfuric acid 180mL, nitric acid 60mL;
3. the stirring magneton in there-necked flask begins 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 the ultra-sonic dispersion instrument, make the oxide solution in there-necked flask be cooled to 25 ℃;
6. suction filtration is placed in oxide solution the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, retains the product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. deionized water wash, suction filtration
The product filter 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, retain the 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 with the product filter cake and carries out drying, 80 ℃ ± 2 ℃ of drying temperatures, and vacuum tightness 10Pa, time of drying 8, h, got 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;
2. open the electric heating agitator, 70 ℃ ± 2 ℃ of Heating temperatures, and stir;
3. heat, stir 24 h, carry out the modification reaction;
4. in the reaction of chloride modification, chemical reaction will occur, reaction formula is as follows:
In formula:
C-COCl: chloride carbon nanotube
SO
2: sulfurous gas
5. after modification, modified-reaction, close the electric heating agitator, stopped heating stirs, and makes it be cooled to 25 ℃ with bottle: modification solution;
6. suction filtration is placed in modification solution the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, retains the product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. tetrahydrofuran (THF) washing, suction filtration
The product filter 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, retain the product filter cake on filter membrane, washings is evacuated in filter flask;
Tetrahydrofuran (THF) washing, suction filtration to filtrate are clarified;
8. vacuum-drying is placed in vacuum drying oven with the product filter cake and carries out drying, 80 ℃ ± 2 ℃ of drying temperatures, and vacuum tightness 10Pa, time of drying 8, h, got after drying: the 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;
2. open the electric heating agitator, 100 ℃ ± 2 ℃ of oil bath cylinder Heating temperatures, and stir;
3. constant temperature stirs 48 h, carries out aminated reaction; ,
4. in aminated reaction, chemical reaction will occur, reaction formula is as follows:
In formula:
C-CONH (CH
2)
2NH
2: aminated carbon nanotube
HCl: hydrogenchloride
5. after the reaction, close the electric heating agitator, stop stirring, make it be cooled to 25 ℃ with bottle: aminated solution;
6. suction filtration is placed in aminated solution the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, retains the product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. absolute ethanol washing, suction filtration
The product filter 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, retain the 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 with the product filter cake and carries out drying, 80 ℃ ± 2 ℃ of drying temperatures, and vacuum tightness 10Pa, time of drying 8, h, got after drying: the carbon nanotube of aminated modification;
(6) preparation carbon nano tube/polyamide 6 amine 66 matrix materials
1. vacuum-drying, with polyamide 66,60g ± 0.001g carries out vacuum-drying dehydration in vacuum drying oven, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 10Pa, time of drying 12 h;
2. extruding pelletization
With polyamide 66,60g ± 0.0001g, aminated carbon nanotube 1.5g ± 0.001g joins in compounding extruder, mixes;
The forcing machine Heating temperature is 260 ℃ ± 5 ℃, squeeze pressure 45MPa, extruding 5s interval time, polyamide 66, aminated carbon nanotube mixture are added in twin screw extruder, extrudate is cooling through cooling trough, the dicing machine cutting, becomes particulate state, particle diameter≤Φ 1mm, length≤5mm;
After extruding be: carbon nano tube/polyamide 6 amine 66 matrix materials;
(7) vacuum-drying, dehydration
Carbon nano tube/polyamide 6 amine 66 particles are carried out drying and dehydrating in vacuum drying oven, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 10Pa, time of drying 12 h;
(8) detect, analyze, characterize
Pattern, structure, composition, chemical physics performance, the frictional behaviour of carbon nano tube/polyamide 6 amine 66 matrix materials to preparation detects, analyzes, characterizes;
Carry out morphology analysis with field emission scanning electron microscope;
Carry out the surface functional group analysis with infrared spectrometer;
Carry out the crystalline texture analysis with X-ray diffractometer;
Carry out thermal stability analysis with thermogravimetric analyzer;
Carry out the crystallinity analysis with differential scanning calorimeter;
Carry out mechanics property analysis with omnipotent tensilometer;
Carry out the Micro Mechanical Properties analysis with nano-hardness tester;
Carry out Analysis on Friction Performance with frictional testing machines;
Conclusion: carbon nano tube/polyamide 6 amine 66 matrix materials are the dark circles cylindrical particle, particle diameter≤Φ 1mm, length≤5mm, and smooth surface, the frictional coefficient of its matrix material reduces by 0.1;
(9) product stores
Carbon nano tube/polyamide 6 amine 66 matrix materials to preparation are stored in brown transparent glass container, and airtight keeping in Dark Place wants waterproof, sun-proof, moistureproof, anti-acid-alkali salt to corrode, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
Beneficial effect
the present invention compares with background technology has obvious advance, adopted brand-new preparation technology's flow process, first carbon nanotube is carried out oxidation, chloride, aminated processing, by melt blending synthesizing carbon nanotubes/polyamide 66 composite material, through the extruding pelletization melting mixing, even carbon nanotube is dispersed in the polyamide 66 matrix, obtain finely dispersed matrix material, improved the intensity of polyamide 66, high temperature resistant, anti-oxidant, erosion resistance, and can reduce the frictional coefficient of matrix material, this preparation method's technique is tight, rationally advanced, informative data is accurate, product quality is good, the polyamide 66 of preparation can be used at multiple industrial circle, the enhancing preparation method of very good polyamide 66 composite material.
Description of drawings
Fig. 1 is the 66 extruding pelletization state graphs of carbon nano tube/polyamide 6 amine
Fig. 2 is that carbon nano tube/polyamide 6 amine 66 matrix materials amplify 10000 times of scanning shape appearance figures
Fig. 3 is carbon nano tube/polyamide 6 amine 66 composite materials property graphic representations
Fig. 4 is that carbon nano tube/polyamide 6 amine 66 matrix material tension fracture faces amplify 10000 scanning shape appearance figures
Fig. 5 is the frictional behaviour graphic representation of carbon nano tube/polyamide 6 amine 66 matrix materials
Shown in figure, list of numerals is as follows:
1. the extruding support, 2. push 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 heater, 14. electric control boxs, 15. display screens; 16. pilot lamp, 17. extruding motor modulators, 18. air dryer modulators; 19. the dicing machine modulator, 20. well heater modulators, 21. wires.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, be the 66 extruder grain state graphs of carbon nano tube/polyamide 6 amine, each position, annexation will be correctly, proportioning, operation according to the order of sequence according to quantity.
The value of the chemical substance that preparation is used is to determine by the scope that sets in advance, take gram, milliliter as measure unit.
The extruder grain moulding of carbon nano tube/polyamide 6 amine 66 matrix materials is carried out on extrusion machine, completes in batch mixing, heating, extrusion screw extruding, cooling, air-dry, pelletizing process;
Extrusion machine is horizontal, left part at extruding support 1 is extruding motor 2, feed sleeve 3 on the right part connection extruder seat 1 of extruding motor 2, feed sleeve 3 right parts connect extrusion screw sleeve 4, extrusion screw sleeve 4 right parts connect cooling tank 5 and cooling trough 6, and cooling tank 5 right parts connect air dryer 7, and air dryer 7 right parts connect dicing machine 8, dicing machine 8 right parts are discharge port 9, and discharge port 9 is aimed 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; Left part at extruding motor 2 is electric control box 14; display screen 15, pilot lamp 16, extruding motor modulator 17, air dryer modulator 18, dicing machine modulator 19 are set on electric control box 14, 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 Figure 2, be carbon nano tube/polyamide 6 amine 66 matrix material shape appearance figures, in figure as can be known: white bright spot is carbon nanotube, evenly minute in the polyamide 66 matrix, ruler units 1 μ m.
Shown in Figure 3, be carbon nano tube/polyamide 6 amine 66 composite materials property graphic representations, ordinate zou is that stress intensity, X-coordinate are strain value, the a curve is the stress-strain(ed) curve of polyamide 66, the b curve is the stress-strain(ed) curve of carbon nano tube/polyamide 6 amine 66 matrix materials, the tensile strength of matrix material b has improved 12.7%, and modulus has improved 24.2%, and the mechanical property of matrix material obviously improves.
Shown in Figure 4, for amination carbon nano tube/polyamide 6 amine 66 matrix material tension fracture faces amplify 10000 times of scanning shape appearance figures, in figure as can be known: the amination even carbon nanotube is dispersed in the polyamide 66 matrix, and carbon nanotube is drawn out from the polyamide 66 matrix at the surface of fracture place, ruler units 1 μ m.
Shown in Figure 5, frictional behaviour graphic representation for carbon nano tube/polyamide 6 amine 66 matrix materials, ordinate zou is that frictional coefficient, X-coordinate are wearing-in period, the c curve is the frictional coefficient curve of polyamide 66, the d curve is the frictional coefficient curve of carbon nano tube/polyamide 6 amine 66 matrix materials, the average friction coefficient of matrix material d has reduced by 0.1, and the frictional behaviour of matrix material obviously improves.
Claims (2)
1. carbon nano tube/polyamide 6 amine 66 composite manufacture methods, 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 consumption is prepared in its combination: take gram, milliliter as 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
The preparation method is as follows:
(1) selected chemical substance material
The chemical substance material that preparation is used will carry out selected, and carry out quality purity, concentration is controlled:
Carbon nanotube: solid-state solid diameter≤Φ 50 nm, length≤20 μ m, purity＞99 %
Polyamide 66: solid-state solid, 99%
Sulfuric acid: liquid strength of fluid 98%
Nitric acid: liquid strength of fluid 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, the thinning processing carbon nanotube
Carbon nanotube is ground with agate mortar, pestle, then sieve with 650 eye mesh screens, grind, sieve and repeatedly carry out;
(3) oxide treatment carbon nanotube
The oxide treatment carbon nanotube carries out on there-necked flask, ultra-sonic dispersion instrument, completes under ultrasonic water heating, stirring;
1. take carbon nanotube 3g ± 0.001g, add in there-necked flask, then be placed on the ultra-sonic dispersion instrument;
2. open the ultra-sonic dispersion instrument, under ultrasonic frequency 50kHz, 50 ℃ ± 2 ℃ of Heating temperatures add sulfuric acid 180mL, nitric acid 60mL;
3. the stirring magneton in there-necked flask begins 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 the ultra-sonic dispersion instrument, make the oxide solution in there-necked flask be cooled to 25 ℃;
6. suction filtration is placed in oxide solution the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, retains the product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. deionized water wash, suction filtration
The product filter 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, retain the 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 with the product filter cake and carries out drying, 80 ℃ ± 2 ℃ of drying temperatures, and vacuum tightness 10Pa, time of drying 8, h, got 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 are added in there-necked flask;
Sulfur oxychloride 100 mL are added in there-necked flask;
2. open the electric heating agitator, 70 ℃ ± 2 ℃ of Heating temperatures, and stir;
3. heat, stir 24 h, carry out the modification reaction;
4. in the reaction of chloride modification, chemical reaction will occur, reaction formula is as follows:
In formula:
C-COCl: chloride carbon nanotube
SO
2: sulfurous gas
5. after modification, modified-reaction, close the electric heating agitator, stopped heating stirs, and makes it be cooled to 25 ℃ with bottle: modification solution;
6. suction filtration is placed in modification solution the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, retains the product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. tetrahydrofuran (THF) washing, suction filtration
The product filter 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, retain the product filter cake on filter membrane, washings is evacuated in filter flask;
Tetrahydrofuran (THF) washing, suction filtration to filtrate are clarified;
8. vacuum-drying is placed in vacuum drying oven with the product filter cake and carries out drying, 80 ℃ ± 2 ℃ of drying temperatures, and vacuum tightness 10Pa, time of drying 8, h, got after drying: the 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 are added in there-necked flask;
2. open the electric heating agitator, 100 ℃ ± 2 ℃ of oil bath cylinder Heating temperatures, and stir;
3. constant temperature stirs 48 h, carries out aminated reaction; ,
4. in aminated reaction, chemical reaction will occur, reaction formula is as follows:
In formula:
C-CONH (CH
2)
2NH
2: aminated carbon nanotube
HCl: hydrogenchloride
5. after the reaction, close the electric heating agitator, stop stirring, make it be cooled to 25 ℃ with bottle: aminated solution;
6. suction filtration is placed in aminated solution the Büchner funnel of filter flask, carries out suction filtration with millipore filtration, retains the product filter cake on filter membrane, and waste liquid is evacuated in filter flask;
7. absolute ethanol washing, suction filtration
The product filter 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, retain the 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 with the product filter cake and carries out drying, 80 ℃ ± 2 ℃ of drying temperatures, and vacuum tightness 10Pa, time of drying 8, h, got after drying: the carbon nanotube of aminated modification;
(6) preparation carbon nano tube/polyamide 6 amine 66 matrix materials
1. vacuum-drying, with polyamide 66,60g ± 0.001g carries out vacuum-drying dehydration in vacuum drying oven, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 10Pa, time of drying 12 h;
2. extruding pelletization
With polyamide 66,60g ± 0.0001g, aminated carbon nanotube 1.5g ± 0.001g joins in compounding extruder, mixes;
The forcing machine Heating temperature is 260 ℃ ± 5 ℃, squeeze pressure 45MPa, extruding 5s interval time, polyamide 66, aminated carbon nanotube mixture are added in twin screw extruder, extrudate is cooling through cooling trough, the dicing machine cutting, becomes particulate state, particle diameter≤Φ 1mm, length≤5mm;
After extruding be: carbon nano tube/polyamide 6 amine 66 matrix materials;
(7) vacuum-drying, dehydration
Carbon nano tube/polyamide 6 amine 66 particles are carried out drying and dehydrating in vacuum drying oven, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 10Pa, time of drying 12 h;
(8) detect, analyze, characterize
Pattern, structure, composition, chemical physics performance, the frictional behaviour of carbon nano tube/polyamide 6 amine 66 matrix materials to preparation detects, analyzes, characterizes;
Carry out morphology analysis with field emission scanning electron microscope;
Carry out the surface functional group analysis with infrared spectrometer;
Carry out the crystalline texture analysis with X-ray diffractometer;
Carry out thermal stability analysis with thermogravimetric analyzer;
Carry out the crystallinity analysis with differential scanning calorimeter;
Carry out mechanics property analysis with omnipotent tensilometer;
Carry out the Micro Mechanical Properties analysis with nano-hardness tester;
Carry out Analysis on Friction Performance with frictional testing machines;
Conclusion: carbon nano tube/polyamide 6 amine 66 matrix materials are the dark circles cylindrical particle, particle diameter≤Φ 1mm, length≤5mm, and smooth surface, the frictional coefficient of its matrix material reduces by 0.1;
(9) product stores
Carbon nano tube/polyamide 6 amine 66 matrix materials to preparation are stored in brown transparent glass container, and airtight keeping in Dark Place wants waterproof, sun-proof, moistureproof, anti-acid-alkali salt to corrode, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
2. a kind of carbon nano tube/polyamide 6 amine 66 composite manufacture methods according to claim 1, it is characterized in that: the extruder grain moulding of carbon nano tube/polyamide 6 amine 66 matrix materials is carried out on extrusion machine, completes in batch mixing, heating, extrusion screw extruding, cooling, air-dry, pelletizing process;
extrusion machine is horizontal, left part at extruding support (1) is 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) is aimed 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), left part at extruding motor (2) is electric control box (14), display screen (15), pilot lamp (16), extruding motor modulator (17), air dryer modulator (18), dicing machine modulator (19) are set on electric control box (14), 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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| CN107474294A (en) * | 2017-09-07 | 2017-12-15 | 青岛科技大学 | The preparation method and its material of high wear-resistant carbon hydridization polyamide electroconductive composite |
| CN107474294B (en) * | 2017-09-07 | 2020-04-24 | 青岛科技大学 | Preparation method of high-wear-resistance carbon hybrid polyamide conductive composite material and material thereof |
| CN108437261A (en) * | 2018-03-23 | 2018-08-24 | 韦龙生 | A kind of stable type plastic pellet Preparation equipment |
| CN109738476A (en) * | 2019-01-17 | 2019-05-10 | 浙江大学 | A kind of integrated apparatus and method for testing phase-change heat-storage material stability |
| CN111117226A (en) * | 2019-12-30 | 2020-05-08 | 湖南华曙高科技有限责任公司 | Nylon powder for selective laser sintering and preparation method thereof |
| CN111534882A (en) * | 2020-05-22 | 2020-08-14 | 北京光华纺织集团有限公司 | Preparation method of functionalized multi-walled carbon nanotube reinforced polyester fiber |
| CN111534882B (en) * | 2020-05-22 | 2022-05-20 | 北京光华纺织集团有限公司 | Preparation method of functionalized multi-walled carbon nanotube reinforced polyester fiber |
| CN113174121A (en) * | 2021-04-08 | 2021-07-27 | 宁波坚锋新材料有限公司 | Regenerated ABS composite material and preparation method thereof |
| CN113174121B (en) * | 2021-04-08 | 2022-08-05 | 宁波坚锋新材料有限公司 | Regenerated ABS composite material and preparation method thereof |
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