CN109180929A - A kind of antistatic-level graphene nylon 6 composite material preparation method - Google Patents
A kind of antistatic-level graphene nylon 6 composite material preparation method Download PDFInfo
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- CN109180929A CN109180929A CN201810814669.2A CN201810814669A CN109180929A CN 109180929 A CN109180929 A CN 109180929A CN 201810814669 A CN201810814669 A CN 201810814669A CN 109180929 A CN109180929 A CN 109180929A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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Abstract
A kind of antistatic-level graphene nylon 6 composite material preparation method, belongs to field of polymer composite material.Using in-situ copolymerization method, the graphene oxide of high level is added in caprolactam, then the ring-opening polymerisation of caprolactam is carried out, pass through the graft reaction between surface functional group, nylon is grafted on graphene oxide, and graphene oxide is reduced to graphene, to prepare 6 master batch of graphene nylon.Then the method squeezed out using melt blending, which is blended with pure nylon 6 according to a certain percentage, is had excellent performance to prepare, antistatic-level graphene nylon 6 composite material.The graphene nylon 6 composite material involved in the present invention arrived has preferable antistatic property, and production technology of the invention only needs to carry out simple modifications to present technique, is suitble to industrial production.
Description
Technical field
The invention belongs to field of polymer composite material, are related to a kind of antistatic-level graphene nylon 6 composite material preparation
Method, prepared graphene nylon 6 composite material have excellent antistatic property.
Background technique
Polyamide is important one of five large-engineering plastics, is widely used in machinery, ship, automobile, household electrical appliances, aviation, electricity
The fields such as sub- electric appliance.With the rapid development of modern science and technology, product is also higher and higher to the performance requirement of polyamide.Polyamide tool
There is high electrical insulating property, is very easy to generate the accumulation of electrostatic charge in large quantities in production, processing, transportational process, when serious
It but will cause the disasters such as explosion, fire.Therefore, conductive modified is carried out to polyamide to be of great significance.
Nano modified material is an importance of Development of Nanometer Material application, and the nano modified material of formation both had
The toughness and workability of high molecular material, and rigidity and property with nano material.Graphene is after carbon nanotube
Afterwards, the another nanoscale functional material of carbon material family has become materialogy, physics, the world heat of chemical field at present
Point project.Graphene has the advantages that high mechanical strength, electric conductivity is high, and stability is good, and raw material sources enrich, this is graphene Buddhist nun
The research of imperial nanocomposite provides possibility.
With this nano-material modified nylon of graphene, the traditional material that modification of nylon is limited to is breached.Modification mode
Do not use traditional physical blending yet, and be changed to caprolactam in-situ polymerization, very good solution physical blending institute with
The bad problem of dispersion, the functional group of surface of graphene oxide and the highly polar effect of nylon amido bond, so that the two interface
In conjunction with greatly enhancing, the nylon molecules chain of grafting is also improved the compatibility of the two.And in the course of the polymerization process, aoxidize stone
Black alkene is reduced to graphene, and electric conductivity restores.On graphene although a large amount of carboxyl functional group is conducive to the grafting of nylon,
But since carboxyl is the end-capping reagent of nylon, will limit the growth of nylon chain in the course of the polymerization process, cause finally with oxidation stone
The molecular weight of the increase of black alkene content, nylon can gradually lower, and finally will affect the performance of nylon instead in this way.
Graphene nylon master batch is generally prepared using graphene and nylon monomer elder generation reaction in-situ in the prior art, then again
With nylon is compound can overcome the above problem, but still not can be further improved in graphene nylon agglomerate material in the prior art
The molecular weight problem of nylon.In patent 201610475005.9, the graphene of high thermal conductivity described in Qiu et al./nylon composite materials
In, using two sections of heatings, high pressure is kept to react the obtained composite material of in-situ polymerization, can there is that molecular weight is lower to ask
Topic.
A certain amount of nylon molecules chain is grafted in surface of graphene oxide.In subsequent blending process, increase
With the compatibility of nylon matrix, keeps graphene evenly dispersed in nylon matrix, it is compound to prepare High-performance graphene nylon 6
Material.The addition of graphene and the evenly dispersed electric conductivity that nylon material can be greatly improved, to obtain antistatic stone
Black alkene nylon 6 composite material.
Summary of the invention
The purpose of the present invention is to provide a kind of antistatic-level graphene nylon 6 composite material preparation methods, using original position
Copolymerization method adds the graphene oxide of high level in caprolactam, then carries out the ring-opening polymerisation of specific caprolactam
And pass through the graft reaction between surface functional group, nylon is grafted on graphene oxide, and graphene oxide is poly-
It is reduced to graphene during closing, nylon molecular weight distribution is narrower, the higher graphene nylon 6 of molecular weight is female to prepare
Grain.Then the method squeezed out using melt blending, which is blended with pure nylon 6 according to a certain percentage, to prepare
It has excellent performance out, antistatic graphene nylon 6 composite material.
To solve the above problems, the scheme that the present invention takes is as follows:
A kind of antistatic-level graphene nylon 6 composite material preparation method, which is characterized in that comprise the following steps that
(1) the carboxylic graphene oxide water solution in surface is mixed with caprolactam, sonic oscillation is uniformly mixed
Liquid；
(2) product in step (1) is transferred in high-temperature high-pressure reaction kettle, is passed through nitrogen and evacuation cycle operation is more
It is secondary, air in kettle is discharged, high-speed stirred is reacted by certain polymerization technique；
(3) after reaction, product takes out step (2) by water cooling, is extracted in boiling water after crushing；
(4) step (3) products therefrom is taken out, vacuum and heating drying processing is carried out in vacuum drying oven, stone can be obtained
Black 6 master batch of alkene nylon；
(5) step (4) master batch is blended according to certain proportion using double screw extruder with 6 pellet of nylon, i.e.,
High-performance, antistatic graphene nylon 6 composite material can be obtained.
Further, the concentration of step (1) graphene oxide water solution is 0.5-7mg/mL, graphene oxide carbon-to-oxygen ratio 3-
Between 6,200nm-100 μm of lamella single side size, the number of plies is between 1-10 layers；In 6 master batch of graphene nylon, graphene quality
Score is 1-20%, and nylon mass fraction is 99-80%, and ultrasonic temperature is 80-100 DEG C, time 0.5-3h.
Further, polymerization technique described in step (2) are as follows: be warming up to 80-100 DEG C of stirring 1-2h, fill during this process
There is also aqueous solutions in setting；150-190 DEG C of stirring 0.5-1.5h is then heated to, 200-230 DEG C of stirring 0.5-2h is warming up to,
In the above process, the water in aqueous solution all switchs to vapor, and keeping pressure is 2-4MPa；Then steam is drained, is vacuumized,
It is warming up to 250-300 DEG C, reacts 1-4h, pressure release to normal pressure, then vacuumize, keeps 1-8h.
Further, extraction time described in step (3) is preferably 12-96h, changes water and repeats 2-5 times.
Further, preferred 50-100 DEG C of vacuum and heating drying treatment temperature described in step (4), time 12-96h.
Further, water when step (2) is reacted in system causes caprolactam open loop as ring opening agent, then occurs poly-
Reaction is closed, and during nylon chain polymerization, reacts with the carboxyl of surface of graphene oxide, is grafted on graphene oxide
Surface.
Further, the antistatic graphene nylon 6 obtained after master batch and pure nylon 6 mixing described in step (5) is compound
The mass percentage of final graphene is 0.5-10% in material.
Further, extruder temperature described in step (5) is arranged: an area is 180 DEG C -250 DEG C, and-six area of 2nd areas is 200
DEG C -260 DEG C, seven areas-No.12 District is 210 DEG C -300 DEG C, 220 DEG C -300 DEG C of head temperature, screw speed 200-400r/min.
The beneficial effects of the present invention are:
Master batch preparation process of the present invention uses multistage gradient increased temperature: low temperature melts mixing, medium temperature hydrolyzation open loop, stabilising system
Oligomer is generated, high temperature polymerization extends nylon chain.And accurately the pressure in control reaction, when hydrolysis, keep higher
Pressure promotes the generation of hydrolysis reaction and oligomer；But nylon 6/poly can generate water during closing, water is to nylon 6
Further reaction has inhibition, so moisture in kettle is discharged, pressure release to normal pressure, vacuumizes by we in subsequent reaction,
Reaction later is always maintained at negative pressure state, and system is sufficiently discharged in the moisture that reaction generates, promotes the life of 6 strand of nylon
It is long.Then, we have also carried out extraction processing, eliminate unreacted monomer and reduce the oligomer of molecular weight.So comparing
In the method for forefathers, the masterbatch composite material that we prepare molecular weight distribution in identical graphene content is narrower, molecular weight more
Height, viscosity average molecular weigh are maintained between 6000-19000 according to the difference of graphene content.
High graphene content master batch is prepared by in-situ polymerization, in the method squeezed out by melt blending, is not only thoroughly solved
It is the problem of nanometer particle-modified bad dispersibility in the process of having determined, ingenious that the characteristics of nylon 6/poly closes reaction is utilized, in graphite oxide
Fixed 6 strand of nylon is grafted in alkene nanometer sheet, and graphene oxide is reduced to graphene, by the excellent performance of graphene
It is introduced into nylon 6 material；And the negative effect that 6 molecular weight of nylon caused by adding graphene oxide into reduces reduces, thus
It prepares and has excellent performance, antistatic graphene nylon 6 composite material.Meanwhile the process that the present invention uses is not needed to original
There is the equipment of industrialized production nylon 6 to be improved on a large scale, is very suitable for industrialized production.
Specific implementation method
Below according to specific embodiment, the present invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
(1) by lamella single side size 200nm, the carboxylic graphite oxide in the surface that carbon-to-oxygen ratio 3, concentration are 0.5mg/mL
Alkene solution 6L is mixed with 297g caprolactam, and 80 DEG C of sonic oscillation 1h, be uniformly mixed liquid；
(2) product in step (1) is transferred in high-temperature high-pressure reaction kettle, is passed through nitrogen and evacuation cycle operates 3 times,
Air in kettle, high-speed stirred is discharged, polymerization technique is to be warming up to 80 DEG C of stirring 1h；150 DEG C of stirring 0.5h are warming up to, are warming up to
200 DEG C of stirrings 0.5h, steam pressure 2MPa；Then it drains, vacuumizes, be warming up to 250 DEG C, react 1h, pressure release to normal pressure is taken out
Vacuum keeps 1h；
(3) after reaction, product takes out by water cooling, extracts for 24 hours after crushing in boiling water, changes water and be repeated 3 times；
(4) product is taken out, 50 DEG C of vacuum heating treatment 72h in vacuum drying oven.Viscosity average molecular weigh is maintained at 17000 left sides
It is right.
(5) product is blended with a certain amount of pure nylon using double screw extruder, extruder temperature setting: one
Area be 200 DEG C ,-six area of 2nd areas be 220 DEG C, seven areas-No.12 District be 230 DEG C, 240 DEG C of head temperature, screw speed 300r/
min.The graphene nylon 6 composite material that final obtained graphene content is 0.5%.
The antistatic test result of products therefrom sample preparation is as shown in table 1:
Embodiment 2
(1) by 1 μm of lamella single side size, the carboxylic graphene oxide in the surface that carbon-to-oxygen ratio 4, concentration are 3mg/mL is molten
Liquid 2L is mixed with 294g caprolactam, and 90 DEG C of sonic oscillation 0.5h, be uniformly mixed liquid；
(2) product in step (1) is transferred in high-temperature high-pressure reaction kettle, is passed through nitrogen and evacuation cycle operates 3 times,
Air in kettle, high-speed stirred is discharged, polymerization technique is to be warming up to 85 DEG C of stirring 1.5h；190 DEG C of stirring 1.5h are warming up to, are warming up to
230 DEG C of stirrings 2h, steam pressure 3MPa；Then it drains, vacuumizes, be warming up to 270 DEG C, react 2h, pressure release to normal pressure is taken out true
Sky keeps 6h；
(3) after reaction, product takes out by water cooling, extracts 48h in boiling water after crushing, changes water and be repeated 3 times；
(4) product is taken out, 70 DEG C of vacuum heating treatment 48h in vacuum drying oven.Viscosity average molecular weigh is maintained at 15000 left sides
It is right.
(5) product is blended with a certain amount of pure nylon using double screw extruder, extruder temperature setting: one
Area be 180 DEG C ,-six area of 2nd areas be 200 DEG C, seven areas-No.12 District be 210 DEG C, 220 DEG C of head temperature, screw speed 200r/
min.The graphene nylon 6 composite material that final obtained graphene content is 0.7%.
The antistatic test result of products therefrom sample preparation is as shown in table 1:
Embodiment 3
(1) by 10 μm of lamella single side size, the carboxylic graphene oxide in the surface that carbon-to-oxygen ratio 5, concentration are 5mg/mL
Solution 3L is mixed with 285g caprolactam, and 100 DEG C of sonic oscillation 3h, be uniformly mixed liquid；
(2) product in step (1) is transferred in high-temperature high-pressure reaction kettle, is passed through nitrogen and evacuation cycle operates 3 times,
Air in kettle, high-speed stirred is discharged, polymerization technique is to be warming up to 100 DEG C of stirring 2h；160 DEG C of stirring 1h are warming up to, are warming up to 210
DEG C stirring 1h, steam pressure 3MPa；Then it draining, vacuumizes, be warming up to 300 DEG C, react 4h, pressure release to normal pressure vacuumizes,
Keep 8h；
(3) after reaction, product takes out by water cooling, extracts 95h in boiling water after crushing, changes water and be repeated 2 times；
(4) product is taken out, 100 DEG C of vacuum heating treatment 96h in vacuum drying oven.Viscosity average molecular weigh is maintained at 13000
Left and right.
(5) product is blended with a certain amount of pure nylon using double screw extruder, extruder temperature setting: one
Area be 250 DEG C ,-six area of 2nd areas be 260 DEG C, seven areas-No.12 District be 300 DEG C, 300 DEG C of head temperature, screw speed 400r/
min.The graphene nylon 6 composite material that final obtained graphene content is 1%.
The antistatic test result of products therefrom sample preparation is as shown in table 1:
Embodiment 4
(1) by 100 μm of lamella single side size, the carboxylic graphene oxide in the surface that carbon-to-oxygen ratio 6, concentration are 7mg/mL
Solution 8.6L is mixed with 240g caprolactam, and 95 DEG C of sonic oscillation 2h, be uniformly mixed liquid；
(2) product in step (1) is transferred in high-temperature high-pressure reaction kettle, is passed through nitrogen and evacuation cycle operates 3 times,
Air in kettle, high-speed stirred is discharged, polymerization technique is to be warming up to 90 DEG C of stirring 1h；170 DEG C of stirring 1.5h are warming up to, are warming up to
230 DEG C of stirrings 1.5h, steam pressure 4MPa；Then it drains, vacuumizes, be warming up to 270 DEG C, react 3h, pressure release to normal pressure is taken out
Vacuum keeps 6h；
(3) after reaction, product takes out by water cooling, extracts 72h in boiling water after crushing, changes water and be repeated 5 times；
(4) product is taken out, 80 DEG C of vacuum heating treatment 48h in vacuum drying oven；Viscosity average molecular weigh is maintained at 6000 left sides
It is right.
(5) product is blended with a certain amount of pure nylon using double screw extruder, extruder temperature setting: one
Area be 230 DEG C ,-six area of 2nd areas be 230 DEG C, seven areas-No.12 District be 250 DEG C, 250 DEG C of head temperature, screw speed 200r/
min.The graphene nylon 6 composite material that final obtained graphene content is 5%.
The antistatic test result of products therefrom sample preparation is as shown in table 1:
The resulting experimental result of specific 4 embodiments please refers to following table.
Table 1 is the antistatic property test result of graphene nylon 6 composite material prepared by embodiment 1-4.
In conclusion quiet with preferably resisting by the obtained graphene nylon 6 composite material of preparation method of the invention
Electrical property.
Claims (10)
1. a kind of antistatic-level graphene nylon 6 composite material preparation method, which is characterized in that comprise the following steps that
(1) the carboxylic graphene oxide water solution in surface is mixed with caprolactam, sonic oscillation, be uniformly mixed liquid；
Ultrasonic temperature is 80-100 DEG C, time 0.5-3h；
(2) product in step (1) is transferred in high-temperature high-pressure reaction kettle, is passed through nitrogen and evacuation cycle operation repeatedly, row
Air in kettle out, high-speed stirred are reacted by certain polymerization technique；
(3) after reaction, product takes out step (2) by water cooling, is extracted in boiling water after crushing；
(4) step (3) products therefrom is taken out, vacuum and heating drying processing is carried out in vacuum drying oven, graphene can be obtained
6 master batch of nylon；
(5) step (4) master batch is blended according to certain proportion using double screw extruder with 6 pellet of nylon, can be obtained
To high-performance, antistatic graphene nylon 6 composite material；
Polymerization technique described in step (2) are as follows: be warming up to 80-100 DEG C of stirring 1-2h, there is also water-soluble in device during this process
Liquid；150-190 DEG C of stirring 0.5-1.5h is then heated to, 200-230 DEG C of stirring 0.5-2h, in above process, water are warming up to
Water in solution all switchs to vapor, and keeping pressure is 2-4MPa；Then steam is drained, is vacuumized, 250-300 is warming up to
DEG C, 1-4h, pressure release to normal pressure are reacted, then vacuumize, keeps 1-8h.
2. a kind of antistatic-level graphene nylon 6 composite material preparation method described in accordance with the claim 1, which is characterized in that
The concentration of step (1) graphene oxide water solution is 0.5-7mg/mL.
3. a kind of antistatic-level graphene nylon 6 composite material preparation method described in accordance with the claim 1, which is characterized in that
Between graphene oxide carbon-to-oxygen ratio 3-6,200nm-100 μm of lamella single side size, the number of plies is between 1-10 layers.
4. a kind of antistatic-level graphene nylon 6 composite material preparation method described in accordance with the claim 1, which is characterized in that
In 6 master batch of graphene nylon, graphene mass fraction is 1-20%, and nylon mass fraction is 99-80%.
5. a kind of antistatic-level graphene nylon 6 composite material preparation method described in accordance with the claim 1, which is characterized in that
Extraction time described in step (3) is preferably 12-96h, changes water and repeats 2-5 times.
6. a kind of antistatic-level graphene nylon 6 composite material preparation method described in accordance with the claim 1, which is characterized in that
Preferred 50-100 DEG C of vacuum and heating drying treatment temperature, time 12-96h described in step (4).
7. a kind of antistatic-level graphene nylon 6 composite material preparation method described in accordance with the claim 1, which is characterized in that
Water when step (2) is reacted in system causes caprolactam open loop as ring opening agent, polymerization reaction then occurs, and in nylon
During chain polymerization, reacts with the carboxyl of surface of graphene oxide, be grafted on surface of graphene oxide.
8. a kind of antistatic-level graphene nylon 6 composite material preparation method described in accordance with the claim 1, which is characterized in that
Final graphene in the antistatic graphene nylon 6 composite material obtained after master batch described in step (5) and pure nylon 6 mixing
Mass percentage is 0.5-10%.
9. a kind of antistatic-level graphene nylon 6 composite material preparation method described in accordance with the claim 1, which is characterized in that
The setting of extruder temperature described in step (5): an area is 180 DEG C -250 DEG C, and-six area of 2nd areas is 200 DEG C -260 DEG C, seven areas-ten
2nd area be 210 DEG C -300 DEG C, 220 DEG C -300 DEG C of head temperature, screw speed 200-400r/min.
10. a kind of 6 composite wood of antistatic-level graphene nylon being prepared according to the described in any item methods of claim 1-9
Material.
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| CN111471296A (en) * | 2020-01-20 | 2020-07-31 | 江苏华永汽车悬架有限公司 | Manufacturing method of lightweight high-fatigue air spring plastic base |
| CN112851962A (en) * | 2021-01-22 | 2021-05-28 | 江南石墨烯研究院 | Preparation method of composite filler modified nylon |
| CN113956652A (en) * | 2021-12-02 | 2022-01-21 | 厦门凯纳石墨烯技术股份有限公司 | Preparation method of antistatic master batch and antistatic master batch |
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| CN111471296A (en) * | 2020-01-20 | 2020-07-31 | 江苏华永汽车悬架有限公司 | Manufacturing method of lightweight high-fatigue air spring plastic base |
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| CN112851962B (en) * | 2021-01-22 | 2022-04-01 | 江南石墨烯研究院 | Preparation method of composite filler modified nylon |
| CN113956652A (en) * | 2021-12-02 | 2022-01-21 | 厦门凯纳石墨烯技术股份有限公司 | Preparation method of antistatic master batch and antistatic master batch |
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