CN106147295B - A kind of graphene oil slurry and preparation method thereof - Google Patents
A kind of graphene oil slurry and preparation method thereof Download PDFInfo
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- CN106147295B CN106147295B CN201610465194.1A CN201610465194A CN106147295B CN 106147295 B CN106147295 B CN 106147295B CN 201610465194 A CN201610465194 A CN 201610465194A CN 106147295 B CN106147295 B CN 106147295B
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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Abstract
The invention discloses a kind of graphene oil slurry, each component and content are：Solvent 80-90wt%, alkylation modification graphene 5-15wt%, oiliness dispersant 2-7wt%.The present invention provides graphene oil slurry, using alkylation modification agent alkyl chain is accessed in graphene film layer surface, graphene more oleophylic after alkylation modification, then under the action of oiliness dispersant, it is scattered in organic solvent, realizes polymolecularity and stability of the graphene in oil-based solvent.
Description
Technical field
The present invention relates to a kind of high concentration graphene oil slurries, belong to organic/inorganic composite material field.
Background technology
Graphene is one kind by single layer sp2The cellular two-dimensional structure of hexagonal lattice that hydbridized carbon atoms are constituted has very
Excellent mechanical strength (intensity：130GPa, Young's modulus：1TPa), it is widely used in the activeness and quietness of composite material.In addition,
Still most light material, specific surface area are up to 2630m to graphene in the world2/ g meets the light-weighted design requirement of composite material.
Graphene grain size is small, the piece interlayer model ylid bloom action power very strong since conjugated structure is formed so that lamella easily stacks, it is difficult to
Dispersion.Can be water by it with the solvent of dispersed graphite alkene, mainly polar solvent, more other organic polar solvents are easier to divide
It dissipates.Even wanting for current composite material is also not achieved as dispersion solvent, the concentration of obtained stable graphene slurry in water
It asks.And concentration of the graphene in oil-based solvent is lower, stability is worse.
Invention content
The technical problem to be solved by the present invention is to overcome the existing defects, provides a kind of high concentration graphene oiliness slurry
Material, further, the stability of high concentration graphene oil slurry provided by the invention is stronger；
It is a further object of the present invention to provide the preparation methods of above-mentioned graphene oil slurry.
A kind of graphene oil slurry, each component and content are：
Solvent 80-90wt%, alkylation modification graphene 5-15wt%, oiliness dispersant 2-7wt%.
Preferably, above-mentioned graphene oil slurry, each component and content are：
Solvent 85wt%, alkylation modification graphene 10wt%, oiliness dispersant 5wt%.
Preferably, the alkylation modification graphene be single or multi-layer structure graphene powder, piece diameter be 0.2~
10um, thickness are 0.5~30nm, and specific surface area is 200~1000m2/g。
Preferably, the alkylation modification graphene is prepared by the following method：
1) graphite oxide cleavage introduces alkyl chain simultaneously
Dispersant, wetting agent, alkylation modification agent are dissolved in ethyl alcohol, graphite oxide is added, obtains graphite oxide
Suspension, then by suspension be placed in mulser to graphite oxide carry out mechanical stripping, graphite oxide stripping cleavage it is same
When with alkyl chain carry out graft reaction, formed and be grafted with the graphene oxide solution of alkyl chain；
2) low temperature original is also
The graphene oxide solution for being grafted with alkyl chain obtained in step 1) is filtered, is washed, by filter cake in 300
DEG C or less reduction, obtain the graphene powder of alkylation modification.
Preferably, dispersant：Wetting agent：The mass ratio of alkylation modification agent is (0.8~1.5)：(0.02~0.2)：1,
This ratio further preferred 1：0.1：1.
Preferably, the alkylation modification agent：The mass ratio of ethyl alcohol is 1：(90~100), further preferred 1：97.
Preferably, the addition of the graphite oxide and the mass ratio of alkylation modification agent are 1：(0.7~3), preferably
1：1；It is further preferred that the graphite oxide is graphite oxide powder.
Preferably, the aqueous dispersion is the various aqueous dispersants such as PSS, SDBS, SDS, commercialization BYK, AFCONA,
Further preferred PSS.
Preferably, the wetting agent is AFCONA5000.
Preferably, alkylation modification agent is octadecylamine, silane coupling agent.
Preferably, the mulser is high shear force mulser, and mulser stirs 0.5h, rotating speed 10000rpm.
Preferably, the temperature of the reduction is 180~200 DEG C.Recovery time 5-10min.
Preferably, 5~10min is filtered.
Preferably, the oiliness dispersant is BYK163, BYK165 or AFCONA4000 series.
BYK, BYK163, BYK165 are the product of Bi Ke chemical (German BYK companies), AFCONA4000, AFCONA5000
It is the product of Afcona companies, being well known to those skilled in the art can be commercially available with market.
Preferably, the solvent is one or more combinations in white oil, paraffin oil, decahydronaphthalenes, mineral oil；It is preferred that mine
Object oil.
Preferably, oiliness dispersant is added in solvent, stirring is to dissolving, then alkylation modification is added into solvent
Graphene powder, then mechanical dispersion processing is carried out, the graphene slurry disperseed.
The preparation method of above-mentioned graphene oil slurry, the graphene powder secondary addition in three batches of the alkylation modification,
It is followed successively by 4/10,3/10, the 3/10 of total amount, after the graphene powder complete wetting of preceding a batch of alkylation modification, adds
Next batch.
Preferably, the mechanical dispersion uses homogenous disperse machine or high speed oscillator decentralized processing.
It is further preferred that 2~10m/s of the homogenous disperse machine linear velocity；More preferable 4~6m/s, decentralized processing time
For 0.5h, high speed vibrates unit frequency 500~700 times/min, duration of oscillation 1h.
Advantageous effect of the present invention：
The present invention provides graphene oil slurry, using the graphene for being grafted with alkyl chain, in the effect of oiliness dispersant
Under, it is scattered in organic solvent, graphene is made to be changed into lipophile by hydrophily, improve point of the graphene in oil-based solvent
Dissipate property and dispersion stabilization.The grafting rate of graft modification graphene of the present invention is high, by taking modifying agent is octadecylamine as an example, is contained by N
The height of amount infers the height of grafting rate, and N content is up to 1.5wt%；Using modifying agent as silane coupling agent KH560, contained by Si
The height of amount infers that the height of grafting rate, Si contents are contained using modifying agent as silane coupling agent KH560 by Si up to 2.9wt%
The height of amount infers the height of grafting rate, and Si contents are up to 2.8wt%.By graft modification, graphene is become by water solubility
Oil-soluble, using Multistep feeding method, makes modified graphene adequately be disperseed when prepared by the dispersion of slurry.It, can referring to Fig. 1
To find out, graft modification graphene dispersing solution does not settle in 30 days in the present invention, and dispersion stabilization is strong；Referring to Fig. 2, graphene
It is uniform that the Hegman fineness grind photo of oil slurry can be seen that graphene dispersion.
Description of the drawings：
Fig. 1 is after graphene dispersing solution modified in the present invention is diluted to and settles 30 days at room temperature after various concentration
Photo；
Fig. 2 is the Hegman fineness grind photo of graphene oil slurry of the present invention.
Specific implementation mode：
Following specific examples is further analyzed explanation to the present invention, does not limit protection scope of the present invention.
Embodiment 1
1) graphite oxide cleavage introduces alkyl chain simultaneously
100gPSS, 10gAFCONA5000,100g octadecylamine are dissolved in 9700g ethyl alcohol, graphite oxide is added
100g obtains the suspension of graphite oxide, then suspension is placed in high shear force mulser and carries out mechanical stripping to graphite oxide
From mulser stirs 30min, and rotating speed 10000rpm, for graphite oxide while removing cleavage, octadecylamine is grafted to oxidation stone
On the oxygen-containing group of ink, the graphene oxide dispersion for being grafted with octadecylamine is formed.
2) low temperature original is also
First the graphene oxide solution for being grafted with octadecylamine obtained in step 1) is filtered, filters the time according to actual oxygen
Depending on the viscosity of graphite alkene solution, generally 5-10min filters off solvent, by graphene oxide washes clean, then at 200 DEG C
Thermal reduction obtains the graphene powder of octadecylamine modification.
The graphene powder that gained is modified is the graphene powder of single or multi-layer structure, and piece diameter is 0.2~10um, thick
Degree is 0.5~30nm, and specific surface area is 200~1000m2/g。
3) preparation of oiliness graphene slurry
5g dispersant Bs YK163 is pre-dispersed in 85g mineral oil, 10g warps are gradually added under high-speed shearing machine effect
(the secondary addition in three batches of the graphene powder of alkylation modification, is followed successively by 4/10, the 3/ of total amount to the graphene powder that octadecylamine is modified
10,3/10), high speed vibrating dispersion 1h (vibration frequency is 500-700 times/time) forms oiliness graphene slurry.
Embodiment 2
1) graphite oxide cleavage introduces alkyl chain simultaneously
SDBS 80g, AFCONA5000 20g, silane coupling agent 100g are dissolved in ethyl alcohol 9000g, oxidation is added
Graphite 33g obtains the suspension of graphite oxide, then suspension is placed in high shear force mulser and carries out machinery to graphite oxide
Stripping, mulser stir 0.5h, and rotating speed 10000rpm, while removing cleavage, silane coupling agent is grafted to graphite oxide
On the oxygen-containing group of graphite oxide, the graphene oxide dispersion for being grafted with silane coupling agent is formed.
2) low temperature original is also
First the modified graphene oxide solution obtained in step 1) is filtered, it is molten according to practical graphene oxide to filter the time
Depending on the viscosity of liquid, generally 5-10min filters off solvent, and graphene oxide washes clean is obtained then at 180 DEG C of dry reduction
To modified graphene powder.
The graphene powder that gained is modified is the graphene powder of single or multi-layer structure, and piece diameter is 0.2~10um, thick
Degree is 0.5~30nm, and specific surface area is 200~1000m2/g。
3) preparation of oiliness graphene slurry
2g dispersant Bs YK165 is pre-dispersed in 90g white oils, 15g silane is gradually added under high-speed shearing machine effect
(the secondary addition in three batches of the graphene powder of alkylation modification, is followed successively by 4/10, the 3/ of total amount to the graphene powder that coupling agent is modified
10,3/10), homogenous disperse machine dispersion 0.5h (linear velocity 4m/s) forms oiliness graphene slurry.
Embodiment 3
1) graphite oxide cleavage introduces alkyl chain simultaneously
SDS 150g, AFCONA5000 2g, silane coupling agent 100g are dissolved in ethyl alcohol 10kg, oxidation stone is added
Ink powder body 142g obtains the suspension of graphite oxide, then suspension is placed in high shear force mulser and is carried out to graphite oxide
Mechanical stripping, mulser stir 0.5h, and rotating speed 10000rpm, while removing cleavage, silane coupling agent connects graphite oxide
On branch to the oxygen-containing group of graphite oxide, the graphene oxide dispersion for being grafted with silane chain is formed.
2) low temperature original is also
First the graphene oxide solution for being grafted with silane coupling agent obtained in step 1) is filtered, filters the time according to reality
Depending on the viscosity of border graphene oxide solution, generally 5-10min filters off solvent, by graphene oxide washes clean, then at
150 DEG C of dry reduction, obtain silane coupler modified graphene powder.
The graphene powder that gained is modified is the graphene powder of single or multi-layer structure, and piece diameter is 0.2~10um, thick
Degree is 0.5~30nm, and specific surface area is 200~1000m2/g。
3) preparation of oiliness graphene slurry
7g dispersant As FC0NA4000 is pre-dispersed in 80g paraffin oils, is gradually added under high-speed shearing machine effect
Through silane coupler modified graphene powder, (the secondary addition in three batches of the graphene powder of alkylation modification, is followed successively by total amount to 5g
4/10,3/10,3/10), high speed vibrating dispersion 1h (vibration frequency be 500-700 time/time) formation oiliness graphene slurries.
Embodiment 4
1) graphite oxide cleavage introduces alkyl chain simultaneously
AFCONA 120g, AFCONA5000 10g, silane coupling agent 100g are dissolved in ethyl alcohol 9700g, oxygen is added
Graphite powder 100g obtains the suspension of graphite oxide, then suspension is placed in high shear force mulser to graphite oxide
Mechanical stripping is carried out, mulser stirs 0.5h, rotating speed 10000rpm, and graphite oxide is silane coupled while removing cleavage
Agent is grafted on the oxygen-containing group of graphite oxide, forms the graphene oxide dispersion for being grafted with silane chain.
2) low temperature original is also
First the graphene oxide solution for being grafted with silane coupling agent obtained in step 1) is filtered, filters the time according to reality
Depending on the viscosity of border graphene oxide solution, generally 5-10min filters off solvent, by graphene oxide washes clean, then at
250 DEG C of dry reduction, obtain silane coupler modified graphene powder.
The graphene powder that gained is modified is the graphene powder of single or multi-layer structure, and piece diameter is 0.2~10um, thick
Degree is 0.5~30nm, and specific surface area is 200~1000m2/g。
3) preparation of oiliness graphene slurry
6 dispersant B YK165 are pre-dispersed in the decahydronaphthalene bitter edible plant, 5 are gradually added through silane under high-speed shearing machine effect
(the secondary addition in three batches of the graphene powder of alkylation modification, is followed successively by 4/10, the 3/ of total amount to coupling agent modified graphene powder
10,3/10), high speed vibrating dispersion 1h (vibration frequency is 500-700 times/time) forms oiliness graphene slurry.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although with reference to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution recorded in example is modified or equivalent replacement of some of the technical features.All essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (18)
1. a kind of graphene oil slurry, it is characterised in that：Each component and content are：
Solvent 80-90wt%, alkylation modification graphene 5-15wt%, oiliness dispersant 2-7wt%；
The solvent is white oil or decahydronaphthalenes；
The oiliness dispersant is BYK163,165 or AFCONA4000 series；
The alkylation modification graphene is prepared by the following method：
1) graphite oxide cleavage introduces alkyl chain simultaneously
Dispersant, wetting agent, alkylation modification agent are dissolved in ethyl alcohol, graphite oxide is added, obtains the outstanding of graphite oxide
Supernatant liquid, then by suspension be placed in mulser to graphite oxide carry out mechanical stripping, graphite oxide while remove cleavage and
Modifying agent carries out graft reaction, forms the graphene oxide solution for being grafted with alkyl chain；
2) low-temperature reduction
The graphene oxide solution for being grafted with alkyl chain obtained in step 1) is filtered, is washed, by filter cake in 300 DEG C with
Lower thermal reduction, obtains the graphene powder of alkylation modification；
Wherein, the dispersant：Wetting agent：The mass ratio of alkylation modification agent is (0.8~1.5)：(0.02~0.2)：1, institute
The addition for stating graphite oxide and the mass ratio of alkylation modification agent are 1：(0.7~3).
2. graphene oil slurry according to claim 1, it is characterised in that：Each component and content are：
Solvent 85wt%, alkylation modification graphene 10wt%, oiliness dispersant 5wt%.
3. graphene oil slurry according to claim 1 or 2, it is characterised in that：The alkylation modification graphene is
The graphene powder of single or multi-layer structure, piece diameter are 0.2~10 μm, and thickness is 0.5~30nm, specific surface area 200
~1000m2/g。
4. graphene oil slurry according to claim 1, it is characterised in that：
Dispersant：Wetting agent：The mass ratio of alkylation modification agent is 1：0.1：1.
5. graphene oil slurry according to claim 1, it is characterised in that：The alkylation modification agent：The matter of ethyl alcohol
Amount is than being 1：(90~100).
6. graphene oil slurry according to claim 5, it is characterised in that：The alkylation modification agent：The matter of ethyl alcohol
Amount is than being 1：97.
7. graphene oil slurry according to claim 1, it is characterised in that：The addition and alkyl of the graphite oxide
The mass ratio for changing modifying agent is 1：1.
8. graphene oil slurry according to claim 1, it is characterised in that：The graphite oxide is graphite oxide powder
Body.
9. graphene oil slurry according to claim 1, it is characterised in that：Point in the alkylation modification graphene
Powder is aqueous dispersant.
10. graphene oil slurry according to claim 9, it is characterised in that：In the alkylation modification graphene
Dispersant is PSS, SDBS, SDS, commercialization BYK or AFCONA.
11. graphene oil slurry according to claim 1, it is characterised in that：The wetting agent is AFCONA5000.
12. graphene oil slurry according to claim 1, it is characterised in that：Alkylation modification agent is octadecylamine, silane
Coupling agent.
13. graphene oil slurry according to claim 1, it is characterised in that：The mulser emulsifies for high shear force
Machine, mulser stir 0.5h, rotating speed 10000rpm.
14. graphene oil slurry according to claim 1, it is characterised in that：The temperature of the reduction is 180~200
℃；Time 5min-10min.
15. according to the preparation method of any one of the claim 1-14 graphene oil slurries, it is characterised in that：By oiliness point
Powder is added in solvent, and stirring is extremely dissolved, then the graphene powder of alkylation modification is added into solvent, then carries out machinery point
Dissipate processing, the graphene slurry disperseed.
16. according to the preparation method of graphene oil slurry described in claim 15, it is characterised in that：The alkylation modification
Graphene powder secondary addition in three batches is followed successively by 4/10,3/10, the 3/10 of total amount, the graphite of preceding a batch of alkylation modification
After alkene powder complete wetting, next batch is added.
17. according to the preparation method of graphene oil slurry described in claim 16, it is characterised in that：The mechanical dispersion uses
Homogenous disperse machine or high speed oscillator decentralized processing, the linear velocity of homogenous disperse machine are 2~10m/s, and the decentralized processing time is
0.5h；High speed oscillation unit frequency 500~700 times/min, duration of oscillation 1h.
18. according to the preparation method of graphene oil slurry described in claim 17, it is characterised in that：The homogenous disperse machine
Linear velocity is 4~6m/s.
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| CN106865539B (en) * | 2017-03-01 | 2018-11-27 | 上海昂星科技发展有限公司 | A kind of lipophilic graphene nanometer sheet and its preparation method and application |
| CN109609034A (en) * | 2018-12-24 | 2019-04-12 | 苏州圣瑞赛新材料科技有限公司 | Oiliness tire identification line coating, preparation method and application |
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