CN109913289A - A kind of preparation method of graphene oxide cladding carbosphere composite material - Google Patents
A kind of preparation method of graphene oxide cladding carbosphere composite material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of graphene oxide cladding carbosphere composite material to carry out hydro-thermal reaction in acid condition first using glucose solution as carbon source, and products therefrom is washed repeatedly, filters and obtains carbosphere after drying；Then carbosphere is dissolved in the mixed solution of water and dehydrated alcohol, then the mixed solution of silane coupling agent and dehydrated alcohol is added, it is condensed back and is reacted under room temperature or heating condition, products therefrom is washed repeatedly, filter and obtain modified carbosphere after drying；It adds graphene oxide into DMF again, is ultrasonically treated after activator then is added, obtains graphene oxide solution；Modified carbosphere is added in graphene oxide solution again, ultrasonic treatment obtains uniform mixed solution A；Finally catalyst is added in mixed solution A, is then performed under heating conditions condensing reflux, products therefrom is washed repeatedly, filter and is dried to obtain graphene oxide cladding carbosphere composite material.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to a kind of preparation of graphene oxide cladding carbosphere composite material
Method.
Background technique
With the development of nano material preparation and application technology, the research and development and application of the lubricating additive containing nano material
Have become one of the hot spot studied both at home and abroad.Graphene is with its ultra-thin nano-lamellar structure, excellent heating conduction, self-lubricating
Performance, mechanical property and good chemical stability show great application value in high perofmrnace lubricating oils field.As
Lube oil additive, it is easy to enter frictional interface, the stable physical isolation film of formation prevents directly connecing for friction surface
Touching, so that the bearing capacity of lubricating oil and extreme pressure and antiwear behavior be made to be enhanced.But since the specific surface of graphene is big, carbon-coating it
Between interact it is strong, it is poor with base oil interaction force, it is easy to reunite, therefore, it is difficult to long-time stables to be scattered in profit
In lubrication prescription, it is greatly unfavorable to bring for its application.And the graphene oxide as Graphene derivative, it is found that it has the stone that matches in excellence or beauty
The excellent properties of black alkene, oxygen-containing functional group abundant, unique two-dimensional slice structure, ultralow coefficient of friction, superpower hardness,
And outstanding corrosion-resistant and antioxygenic property.Moreover, graphene oxide is easier to functionalization, and prepares compared with graphene
There are many simple process.But the strongly hydrophilic of graphene oxide, cause it can not much there are commonly in solvent stablize point
Dissipate, this for graphene oxide the fields such as composite processing application bring certain obstacle.In order to preferably utilize oxidation
Graphene enriches the function of graphene oxide and dispersed in organic solvent, is usually surface modified to it and surface
Functionalization keeps it preferably compound with basis material.Wherein, carbosphere with its perfect spherical structure, excellent heat resistance and
Chemical stability can serve as a nanometer ball action, and physical separation is generated between contact interface, by sliding friction certain degree
Be converted into rolling friction, play the effect of lubrication and antifriction, and there are " self-healing properties ".Graphene oxide coats carbosphere
Composite material is added in lubricating oil mainly as nanometer additive, reduces coefficient of friction and wear rate, and pass through graphite oxide
The phenomenon that heat generated in friction process is timely spread well, alleviates hot-spot by alkene excellent heating conduction,
The stability and service life of elevating mechanism.Document 1 " in the Chinese patent of Publication No. CN102544459A " discloses one kind
Graphene oxide coat carbosphere composite material and preparation method, the component of material include: hydro-thermal method preparation carbosphere and
The graphene oxide of graphite oxide chemistry method of stripping preparation.Experimental method is, with glucose, sucrose or starch are that carbon source prepares carbon
Dried carbosphere is added in graphene oxide solution and is made into mixed solution by microballoon by graphene oxide wiring solution-forming,
Ultrasound filters and obtains graphene oxide cladding carbosphere composite material after drying.But its composite material prepared is not to answer
For lubricating area, and the composite material in document 1 is combined together by electrostatic interaction, and binding force is weaker, and pattern is not
Regular, there are more defects, is not appropriate for being added in lubricant as nanoparticle additives.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of graphene oxide cladding carbosphere composite material, to overcome
Defect of the existing technology, graphene oxide prepared by the present invention cladding carbosphere composite material can in friction process,
Reduce mechanical coefficient of friction and wear rate, and then prolonged mechanical service life.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of graphene oxide cladding carbosphere composite material, comprising the following steps:
1) using glucose solution as carbon source, hydro-thermal reaction is carried out in acid condition, repeatedly, then products therefrom is washed
It filters and obtains carbosphere after drying；
2) carbosphere is dissolved in the mixed solution of water and dehydrated alcohol, silane coupling agent and dehydrated alcohol is then added
Mixed solution is reacted or is performed under heating conditions condensing reflux reaction in room temperature, repeatedly, then products therefrom is washed
It filters and obtains modified carbosphere after drying；
3) it adds graphene oxide into DMF, is ultrasonically treated, obtain graphene oxide solution；
4) modified carbosphere is added in graphene oxide solution, ultrasonic treatment obtains uniform mixed solution A；
5) catalyst is added in mixed solution A, is reacted or be performed under heating conditions condensing reflux in room temperature
Reaction washs products therefrom repeatedly, filters and is dried to obtain graphene oxide cladding carbosphere composite material.
Further, glucose concentration is 50mg/mL in step 1), and is adjusted by oxalic acid to acidity in step 1)
Condition.
Further, the temperature of hydro-thermal reaction is 180 DEG C in step 1), time 12h.
Further, in step 2) in the mixed solution of deionized water and dehydrated alcohol deionized water and dehydrated alcohol body
0.2g carbosphere is added than being 5:4 in product in the mixed solution of every 180mL deionized water and dehydrated alcohol.
Further, silane coupling agent uses KH550, the mixed solution tool of silane coupling agent and dehydrated alcohol in step 2)
Body are as follows: 0.6g silane coupling agent is added in every 20mL dehydrated alcohol；And the mass ratio of carbosphere and silane coupling agent is 1:3.
Further, 12h is reacted in step 2) at room temperature, or is condensed back 12h at 60 DEG C.
Further, graphene oxide solution concentration is 0.2mg/mL-0.4mg/mL in step 3).
Further, the mass ratio of modified carbosphere and graphene oxide is (1-2) in step 4): 1.
Further, catalyst is HATU in step 5), and the mass ratio of catalyst and modified carbosphere is (1-2): (2-
4)。
Further, it is reacted at room temperature in step 5) for 24 hours, or be condensed back for 24 hours at 60 DEG C.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention is modified carbosphere using chemical method, then by amidation process that graphene oxide is compound with carbosphere.
By observation and analysis, graphene oxide is coated on carbosphere surface, in friction process, a part of graphene oxide of outer layer
The roughness for, into friction area, reducing surface of friction pair with stably depositing can be permeated, directly connecing between slidingsurface is avoided
The phenomenon that touching, and the even heat generated in friction process dissipated, hot-spot is avoided.Carbosphere then acts as bearing,
So that sliding friction dress becomes rolling friction, the lesser carbosphere of size can also be filled into the recess of surface of friction pair, centainly
Play the role of selfreparing in degree.The method gives full play to the synergistic effect of carbosphere and graphene oxide, is effectively improved
The problem of composite material binding force is weak, and pattern is irregular and bad dispersibility.Coefficient of friction and wear rate is greatly lowered, improves
Stability and mechanical service life
Compared with prior art, it is multiple to prepare graphene oxide cladding carbosphere using chemically combined method for the first time by the present invention
Condensation material.Processing is modified to carbosphere using silane coupling agent first, is mentioned for next and graphene oxide combination
Prerequisite, while the alkane chain long by grafting have been supplied, so that it has good dispersibility in organic solvent, and has been had
There is the features such as easy to operate, low for equipment requirements.Secondly graphene oxide and carbosphere are combined by amido bond, than passing through electrostatic
In conjunction with method combine can it is stronger, showed in friction process more stable.Furthermore graphene oxide adheres in friction process
It in surface of friction pair, plays a very good protection, greatly reduces wear rate, be conducive to improve mechanical service life
Performance is raw material using hydro-thermal carbosphere, and raw material sources are extensive, more environmentally friendly, is in a word a kind of green and process control
Preparation method.
Detailed description of the invention
Fig. 1 is the SEM photograph comparison diagram of rear carbosphere before modified, wherein (a) is unmodified carbosphere microscopic appearance,
(b) it is the microscopic appearance of modified carbosphere, (c) is the microscopic appearance of composite material；
The TEM photo of Fig. 2 sample, wherein (a) is modified carbosphere, it (b) is composite material；
Fig. 3 is revolving speed when being 400R, changes the dynamic friction coefficient consecutive variations figure for the sample that pressure obtains, wherein (a) is
3N (b) is 5N, (c) is 8N；
Fig. 4 be original oil, carbosphere, graphene oxide and graphene oxide coat carbosphere composite material in 3N, 5N and
Dynamic friction coefficient figure under 8N；
Fig. 5 is the metallographic microscope photo of steel base after friction, wherein (a) is original oil, it (b) is to be added to 0.2%wt
Carbosphere；(c) (d) multiple to be added to 0.2%wt graphene oxide cladding carbosphere to be added to 0.2%wt graphene oxide
Condensation material.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of preparation method of graphene oxide cladding carbosphere composite material, comprising the following steps:
1) it using glucose solution as carbon source, is carried out after being adjusted by oxalic acid to acid condition, it is anti-in 180 DEG C of progress hot water thermals
12h is answered, products therefrom is washed repeatedly, filters and obtains carbosphere after drying；Wherein glucose concentration is 50mg/mL；
2) carbosphere is dissolved in the mixed solution (deionized water and the volume ratio of dehydrated alcohol be 5:4) of water and dehydrated alcohol
In, and in the mixed solution of every 180mL deionized water and dehydrated alcohol be added 0.2g carbosphere, then be added silane coupling agent and
The mixed solution (in every 20mL dehydrated alcohol be added 0.6g silane coupling agent) of dehydrated alcohol, and carbosphere and silane coupling agent
Mass ratio is 1:3, then carries out reaction 12h under the conditions of room temperature or condensing reflux heating (60 DEG C), products therefrom is washed more
It is secondary, it filters and obtains modified carbosphere after drying；
3) it adds graphene oxide into DMF, ultrasound 1h under the conditions of 60 DEG C, obtaining concentration is 0.2mg/mL-
The graphene oxide solution of 0.4mg/mL；
4) modified carbosphere being added in graphene oxide solution, ultrasonic treatment obtains uniform mixed solution A, wherein
The mass ratio of modified carbosphere and graphene oxide is (1-2): 1；
5) catalyst HATU is added in mixed solution A, the mass ratio for meeting catalyst and modified carbosphere is (1-
2): (2-4) then reacts for 24 hours at room temperature, or is condensed back for 24 hours under 60 DEG C of heating conditions, products therefrom is washed more
It is secondary, graphene oxide cladding carbosphere composite material is dried to obtain after suction filtration.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
1) concentration of configuration glucose and oxalic acid mixed solution, glucose and oxalic acid distinguishes 50mg/ml and 2.5mg/ml,
Product is washed repeatedly, is filtered by 180 DEG C of progress hot water thermal response 12h, obtains carbosphere after dry 12h in 80 DEG C of baking ovens；
2) dry 0.2g carbosphere is dissolved in the mixed solution of 100ml deionized water and 80ml dehydrated alcohol, is added
The mixed solution that 0.6g silane coupling agent and 20ml dehydrated alcohol are equipped with, reacts 12h under the conditions of 60 DEG C of condensing refluxes, by product
Washing repeatedly, filters, and modified carbosphere is obtained after 80 DEG C of oven drying 12h；
3) 30mg graphene oxide is added in 100mlDMF, obtains graphene oxide solution, graphene oxide uses
The preparation of Hummers method；
4) the modified carbosphere of dry 40mg is added in graphene oxide solution, it is molten that ultrasonic 1h obtains uniform mixing
Liquid A；
5) 20mgHATU is added in mixed solution A, under the conditions of 60 DEG C, is condensed back 24 hours, product is multiple
Washing filters, and 80 DEG C of vacuum drying 12h obtain graphene oxide cladding carbosphere composite material.
Embodiment 2
1) concentration of configuration glucose and oxalic acid mixed solution, glucose and oxalic acid distinguishes 50mg/ml and 2.5mg/ml,
Product is washed repeatedly, is filtered by 180 DEG C of progress hot water thermal response 12h, obtains carbosphere after dry 12h in 80 DEG C of baking ovens；
2) dry 0.2g carbosphere is dissolved in the mixed solution of 100ml deionized water and 80ml dehydrated alcohol, is added
The mixed solution that 0.6g silane coupling agent and 20ml dehydrated alcohol are equipped with, reacts 12h under the conditions of 60 DEG C of condensing refluxes, by product
Washing repeatedly, filters, and modified carbosphere is obtained after 80 DEG C of oven drying 12h；
3) 40mg graphene oxide is added in 100mlDMF, obtains graphene oxide solution, graphene oxide uses
The preparation of Hummers method；
4) the modified carbosphere of dry 40mg is added in graphene oxide solution, it is molten that ultrasonic 1h obtains uniform mixing
Liquid A；
5) 40mgHATU is added in mixed solution A, at room temperature, for 24 hours, product is repeatedly washed for reaction, is taken out
Filter, 80 DEG C of vacuum drying 12h obtain graphene oxide cladding carbosphere composite material.
Embodiment 3
1) concentration of configuration glucose and oxalic acid mixed solution, glucose and oxalic acid distinguishes 50mg/ml and 2.5mg/ml,
Product is washed repeatedly, is filtered by 180 DEG C of progress hot water thermal response 12h, obtains carbosphere after dry 12h in 80 DEG C of baking ovens；
2) dry 0.2g carbosphere is dissolved in the mixed solution of 100ml deionized water and 80ml dehydrated alcohol, is added
The mixed solution that 0.6g silane coupling agent and 20ml dehydrated alcohol are equipped with, reacts for 24 hours under the conditions of 60 DEG C of condensing refluxes, by product
Washing repeatedly, filters, and modified carbosphere is obtained after 80 DEG C of oven drying 12h；
3) 30mg graphene oxide is added in 100mlDMF, obtains graphene oxide solution, graphene oxide uses
The preparation of Hummers method；
4) the modified carbosphere of dry 40mg is added in graphene oxide solution, it is molten that ultrasonic 1h obtains uniform mixing
Liquid A；
5) 10mgHATU is added in mixed solution A, under the conditions of 60 DEG C, is condensed back 24 hours, product is multiple
Washing filters, and 80 DEG C of vacuum drying 12h obtain graphene oxide cladding carbosphere composite material.
Embodiment 4
1) concentration of configuration glucose and oxalic acid mixed solution, glucose and oxalic acid distinguishes 50mg/ml and 2.5mg/ml,
Product is washed repeatedly, is filtered by 180 DEG C of progress hot water thermal response 12h, obtains carbosphere after dry 12h in 80 DEG C of baking ovens；
2) dry 0.2g carbosphere is dissolved in the mixed solution of 100ml deionized water and 80ml dehydrated alcohol, is added
The mixed solution that 0.6g silane coupling agent and 20ml dehydrated alcohol are equipped with, reacts for 24 hours under the conditions of 60 DEG C of condensing refluxes, by product
Washing repeatedly, filters, and modified carbosphere is obtained after 80 DEG C of oven drying 12h；
3) 40mg graphene oxide is added in 100mlDMF, obtains graphene oxide solution, graphene oxide uses
The preparation of Hummers method；
4) the modified carbosphere of dry 40mg is added in graphene oxide solution, it is molten that ultrasonic 1h obtains uniform mixing
Liquid A；
5) 10mgHATU is added in mixed solution A, under the conditions of 60 DEG C, is condensed back 24 hours, product is multiple
Washing filters, and 80 DEG C of vacuum drying 12h obtain graphene oxide cladding carbosphere composite material.
Embodiment 5
1) concentration of configuration glucose and oxalic acid mixed solution, glucose and oxalic acid distinguishes 50mg/ml and 2.5mg/ml,
Product is washed repeatedly, is filtered by 180 DEG C of progress hot water thermal response 12h, obtains carbosphere after dry 12h in 80 DEG C of baking ovens；
2) dry 0.2g carbosphere is dissolved in the mixed solution of 100ml deionized water and 80ml dehydrated alcohol, is added
The mixed solution that 0.6g silane coupling agent and 20ml dehydrated alcohol are equipped with, reacts 12h at room temperature, and product is washed repeatedly, is taken out
It filters, modified carbosphere is obtained after 80 DEG C of oven drying 12h；
3) 20mg graphene oxide is added in 100mlDMF, obtains graphene oxide solution, graphene oxide uses
The preparation of Hummers method；
4) the modified carbosphere of dry 40mg is added in graphene oxide solution, it is molten that ultrasonic 1h obtains uniform mixing
Liquid A；
5) 20mgHATU is added in mixed solution A, at room temperature, reacts 24 hours, product is repeatedly washed, takes out
Filter, 80 DEG C of vacuum drying 12h obtain graphene oxide cladding carbosphere composite material.
Comparison is obtained by embodiment 1 from Fig. 1 original carbosphere and silane coupler modified treated carbosphere,
It can be seen that silane coupling agent has successfully been grafted to carbosphere surface by the method for modifying that the present invention uses；It observes modified
Carbosphere and graphene oxide/carbosphere composite material are it is found that the method that the present invention prepares composite material, successfully by graphite oxide
Alkene and carbosphere are combined togather, and graphene oxide is coated on carbosphere surface.
The modified carbosphere and graphene oxide/carbosphere composite material obtained from Fig. 2 by embodiment 1 can
Know that graphene oxide is wrapped in carbosphere surface.
From paired observation in Fig. 3 it is found that the present invention rubs after being added to lubricating oil by composite material prepared by embodiment 1
Coefficient is more stable, and the lubricating oil of coefficient of friction two kinds of materials of addition lower than original oil and individually, illustrates that composite material has
There is better antifriction performance.
As can be seen from Figure 4 revolving speed is that 400R is constant, with the variation of pressure, individually adds the lubricating oil of two kinds of materials
The variation of pressure is become apparent with original oil, after the present invention is added to lubricating oil by composite material prepared by embodiment 1
Coefficient of friction is more stable.
As can be seen from Figure 5 the composite material that the present invention is prepared by embodiment 1 is compared to two kinds of materials of independent addition
Lubricating oil and original oil polishing scratch it is more shallow narrower, illustrate more preferable using the wear resistance of the invention for preparing composite material.
Claims (10)
1. a kind of preparation method of graphene oxide cladding carbosphere composite material, which comprises the following steps:
1) using glucose solution as carbon source, hydro-thermal reaction is carried out in acid condition, and products therefrom is washed repeatedly, is then filtered
And carbosphere is obtained after drying；
2) carbosphere is dissolved in the mixed solution of water and dehydrated alcohol, the mixing of silane coupling agent and dehydrated alcohol is then added
Solution is reacted or is performed under heating conditions condensing reflux reaction in room temperature, products therefrom is washed repeatedly, is then filtered
And modified carbosphere is obtained after drying；
3) it adds graphene oxide into DMF, is ultrasonically treated, obtain graphene oxide solution；
4) modified carbosphere is added in graphene oxide solution, ultrasonic treatment obtains uniform mixed solution A；
5) catalyst is added in mixed solution A, is reacted or be performed under heating conditions condensing reflux reaction in room temperature,
Repeatedly by products therefrom washing, it filters and is dried to obtain graphene oxide cladding carbosphere composite material.
2. a kind of preparation method of graphene oxide cladding carbosphere composite material according to claim 1, feature exist
In glucose concentration is 50mg/mL in step 1), and is adjusted by oxalic acid to acid condition in step 1).
3. a kind of preparation method of graphene oxide cladding carbosphere composite material according to claim 1, feature exist
In the temperature of hydro-thermal reaction is 180 DEG C in step 1), time 12h.
4. a kind of preparation method of graphene oxide cladding carbosphere composite material according to claim 1, feature exist
In deionized water and the volume ratio of dehydrated alcohol are 5:4 in the mixed solution of deionized water and dehydrated alcohol in step 2), and every
0.2g carbosphere is added in the mixed solution of 180mL deionized water and dehydrated alcohol.
5. a kind of preparation method of graphene oxide cladding carbosphere composite material according to claim 4, feature exist
In, in step 2) silane coupling agent use KH550, the mixed solution of silane coupling agent and dehydrated alcohol specifically: every 20mL without
0.6g silane coupling agent is added in water-ethanol；And the mass ratio of carbosphere and silane coupling agent is 1:3.
6. a kind of preparation method of graphene oxide cladding carbosphere composite material according to claim 1, feature exist
In 12h being reacted in step 2) at room temperature, or be condensed back 12h at 60 DEG C.
7. a kind of preparation method of graphene oxide cladding carbosphere composite material according to claim 1, feature exist
In graphene oxide solution concentration is 0.2mg/mL-0.4mg/mL in step 3).
8. a kind of preparation method of graphene oxide cladding carbosphere composite material according to claim 1, feature exist
In the mass ratio of modified carbosphere and graphene oxide is (1-2) in step 4): 1.
9. a kind of preparation method of graphene oxide cladding carbosphere composite material according to claim 1, feature exist
In catalyst is HATU in step 5), and the mass ratio of catalyst and modified carbosphere is (1-2): (2-4).
10. a kind of preparation method of graphene oxide cladding carbosphere composite material according to claim 1, feature exist
In being reacted at room temperature in step 5) for 24 hours, or be condensed back for 24 hours at 60 DEG C.
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| CN111777728A (en) * | 2020-07-10 | 2020-10-16 | 陕西科技大学 | Preparation method of graphene oxide reinforced polymethyl methacrylate/carbon microsphere composite material |
| CN111849585A (en) * | 2020-07-07 | 2020-10-30 | 西安航空职业技术学院 | Preparation method of graphene oxide-polyethylene glycol cross-linked network/carbon microsphere composite material |
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| CN111849585A (en) * | 2020-07-07 | 2020-10-30 | 西安航空职业技术学院 | Preparation method of graphene oxide-polyethylene glycol cross-linked network/carbon microsphere composite material |
| CN111777728A (en) * | 2020-07-10 | 2020-10-16 | 陕西科技大学 | Preparation method of graphene oxide reinforced polymethyl methacrylate/carbon microsphere composite material |
| CN111777728B (en) * | 2020-07-10 | 2022-06-03 | 陕西科技大学 | Preparation method of graphene oxide reinforced polymethyl methacrylate/carbon microsphere composite material |
| CN112898953A (en) * | 2021-01-14 | 2021-06-04 | 蒋军良 | Preparation method of graphene heat-conducting film |
| KR20220103311A (en) * | 2021-01-15 | 2022-07-22 | 성균관대학교산학협력단 | Enhancement structure of the interfacial strength between carbon fiber and epoxy resin composites and manufacturing methode of the same |
| KR102473359B1 (en) * | 2021-01-15 | 2022-12-01 | 성균관대학교산학협력단 | Enhancement structure of the interfacial strength between carbon fiber and epoxy resin composites and manufacturing methode of the same |
| CN113171749A (en) * | 2021-03-16 | 2021-07-27 | 中国工程物理研究院材料研究所 | Magnetic adsorbent for removing uranium plutonium nuclide, preparation method and application |
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