CN110371960A - The stripping means of oily phase graphene and its application - Google Patents
The stripping means of oily phase graphene and its application Download PDFInfo
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- CN110371960A CN110371960A CN201910759684.6A CN201910759684A CN110371960A CN 110371960 A CN110371960 A CN 110371960A CN 201910759684 A CN201910759684 A CN 201910759684A CN 110371960 A CN110371960 A CN 110371960A
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- Prior art keywords
- oil
- agent
- oily phase
- stripping means
- graphene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/22—Intercalation
- C01B32/225—Expansion; Exfoliation
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/02—Carbon; Graphite
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/25—Internal-combustion engines
- C10N2040/255—Gasoline engines
Abstract
The present invention discloses a kind of stripping means of oily phase graphene and its application, method include that natural flake graphite powder is added in base oil and is stirred to form oily phase graphite raw material;It is continuously added expansion in whipping process and tears a layer agent open;3h-5h is stirred, so that the expansion is torn layer agent open and is sufficiently mixed and forms oil mixture between the graphite linings of the oily phase graphite raw material;Chelating is hit in the agent addition oil mixture and stirs evenly to form oily phase reaction object;The oil phase reaction object stands reaction 1-1.5h, forms the oily phase graphene.By the way that natural flake graphite powder is directly added into base oil, dispersion is carried out, it can be by natural flake graphite powder rapid processing at machine oil product, consuming little energy, it can also reduce dry or carry out the molten program of oil with powder, achieve the purpose that reduce cost, save the time and quickly produce.
Description
Technical field
The present invention relates to the stripping means and application of the technical field of graphene more particularly to a kind of oily phase graphene.
Background technique
Oily phase graphene stripping method is based on this paper research group, through many years in graphene research above and using upper experience
It summarizes, it is finally newest in oil phase liquid state environment removing day with one developed on a brand-new design and scientific practice
Right crystalline flake graphite, to reach the graphene applied in oil-soluble material.
In the prior art, the graphene machine oil of manufacture is to carry out the molten processing of oil using the graphene of dry powder to be divided
It dissipates.Passing graphene is produced will also be divided again by dispersing and drying to be made after powder is mixed and dissolved for machine oil
It dissipates, can just obtain the product of being applied to.It can be wasted in the dry process held with rear coming oil of graphene in whole process, increase cost
Add, also brings the increase in overall cost.Asking in the inevitably time-consuming in the whole process and more manpower and material resources of cost
Topic, it is necessary to remove graphene in oily phase and come out application, be only more environmentally friendly and resources economy benefit.
Summary of the invention
Shortcoming present in view of the above technology, the present invention, which provides, a kind of reduces cost, easy to operate oily phase stone
The stripping means of black alkene and application.
In order to achieve the above object, a kind of stripping means of oily phase graphene of the present invention, includes the following steps:
Natural flake graphite powder is added in base oil and is stirred to form oily phase graphite raw material;
It is continuously added expansion in whipping process and tears a layer agent open;
3h-5h is stirred, so that the expansion is torn layer agent open and is sufficiently mixed and is formed between the graphite linings of the oily phase graphite raw material
Oil mixture;
Chelating is hit in the agent addition oil mixture and stirs evenly to form oily phase reaction object;
The oil phase reaction object stands reaction 1-1.5h, forms the oily phase graphene.
Wherein, the size of the natural flake graphite powder is -15000 mesh of 300 mesh.
Wherein, the base oil is basic lubricating oil.
Wherein, the mixed proportion of the natural flake graphite powder and base oil, is calculated, natural flake graphite based on mass fraction
Powder: base oil=1:2.
Wherein, the mixed proportion of layer agent is torn in the oily phase graphite raw material and expansion open, is calculated based on mass fraction, oily phase graphite is former
Material: a layer agent=9:1 is torn in expansion open.
Wherein, the preparation method that layer agent is torn in the expansion open includes the following steps:
By hydrophilic-basic swelling agent and water mixed dissolution, the saturated solution of the hydrophilic-basic swelling agent is formed;
The saturated solution of the hydrophilic-basic swelling agent is added in nonionic chelating agent, by ultrasonic agitation, is formed
A layer agent is torn in the expansion of emulsified state open.
Wherein, the additive amount of the nonionic chelating agent is the mass fraction of the saturated solution of the hydrophilic-basic swelling agent
1%-5%.
Wherein, the hydrophilic-basic swelling agent is one of sodium bicarbonate, precipitated calcium carbonate and sodium peroxide or more
Kind, the nonionic chelating agent is one of EDTA, TDPA and EHDT or a variety of.
Wherein, it is one of EDTA, TDPA and EHDT or a variety of that the chelating, which hits agent, and the chelating hits agent
Additive amount is the 10% of the mass fraction of the oil mixture.
The invention also discloses a kind of application of the stripping means of graphene, the oil phase graphene is added into automobile engine oil
In play lubricating action.
The beneficial effects of the present invention are:
Compared with prior art, this programme carries out dispersion journey by the way that natural flake graphite powder to be directly added into base oil
Sequence, can be by natural flake graphite powder rapid processing at machine oil product, consuming little energy, can also reduce it is dry or with powder into
The molten program of row oil, achievees the purpose that reduce cost, saves the time and quickly produce.
Detailed description of the invention
Fig. 1 is the flow diagram of the stripping means of the oily phase graphene of the present invention;
Fig. 2 is the oily phase graphene performance detection report one of the present invention;
Fig. 3 is the oily phase graphene performance detection report two of the present invention;
Fig. 4 is the oily phase graphene performance detection report three of the present invention;
Fig. 5 is the oily phase graphene performance detection report four of the present invention;
Fig. 6 is the oily phase graphene performance detection report five of the present invention;
Fig. 7 is the oily phase graphene performance detection report six of the present invention.
Specific embodiment
In order to more clearly state the present invention, the present invention is further described with reference to the accompanying drawing.
Refering to fig. 1, a kind of stripping means of oily phase graphene of the present invention, includes the following steps:
Step S10, raw material premix are closed:
Natural flake graphite powder is added in base oil and is stirred to form oily phase graphite raw material;
Step S20 is added expansion and tears a layer agent open:
It is continuously added expansion in whipping process and tears a layer agent open;
A layer agent reaction is torn in step S30, expansion open:
3h-5h is stirred, so that the expansion is torn layer agent open and is sufficiently mixed and is formed between the graphite linings of the oily phase graphite raw material
Oil mixture;
Step S40 is added chelating and hits agent:
Chelating is hit in the agent addition oil mixture and stirs evenly to form oily phase reaction object;
Step S50, reaction generate oily phase graphene:
The oil phase reaction object stands reaction 1-1.5h, forms the oily phase graphene.
Specifically, in step slo, selecting the size of natural flake graphite powder for -15000 mesh of 300 mesh, natural scale stone
Ink powder has many brands in the market, chooses at random the purchase of suitable dimension.The base oil selected is basic lubricating oil,
Base oil can directly be bought from total, SK or other oil product companies.
Natural flake graphite powder and base oil are respectively put into screw blender, natural flake graphite powder and basis
The mixed proportion of oil, is calculated, natural flake graphite powder: base oil=1:2 based on mass fraction.Start screw blender, to turn
The speed that speed is 120r/min rotates, and forms oily phase graphite raw material.In the process, the temperature in screw blender is normal
Temperature, air pressure are an atmospheric pressure.
Specifically, in step S20, when natural crystalline graphite powder and base oil are respectively put into the stirring of screw blender
During, it is continuously added expansion and tears a layer agent open, the mixed proportion of layer agent is torn in oily phase graphite raw material and expansion open, based on mass fraction
Calculate, oily phase graphite raw material: a layer agent=9:1 is torn in expansion open.Expansion is torn layer agent open and is needed using the pollution-free material with side effect, and expansion is torn open
The layer agent gas that generated expansion reaction issues in graphene stripping process must be free of contamination gas, such as titanium dioxide
Carbon or oxygen.
In the present embodiment, hydrophilic-basic swelling agent is one of sodium bicarbonate, precipitated calcium carbonate and sodium peroxide
Or it is a variety of, nonionic chelating agent is one of EDTA, TDPA and EHDT or a variety of.Expansion tears a layer agent open and needs to reach hydrophilic parent
The emulsion state of oil, could fuse in base oil, penetrate between graphite linings.A layer agent release is torn in expansion open during the reaction
Oxygen or carbon dioxide, to open the Van der Waals force of graphite between layers, further to reach the peeling effect of graphite linings.
In the present embodiment, the preparation method that layer agent is torn in expansion open includes the following steps:
Step S21, by hydrophilic-basic swelling agent and water mixed dissolution, the saturation for forming the hydrophilic-basic swelling agent is molten
Liquid.
Hydrophilic-basic swelling agent is sufficiently mixed with water, until hydrophilic-basic swelling agent reaches saturation state, thus may be used
To the full extent using the expansion effect of alkaline swelling agent.
The saturated solution of the hydrophilic-basic swelling agent is added in nonionic chelating agent, is stirred by ultrasound by step S22
It mixes, a layer agent is torn in the expansion for forming emulsified state open.
The saturated solution and nonionic chelating agent of hydrophilic-basic swelling agent are put into ultrasonic stirrer, pass through ultrasonic power
Realize being sufficiently mixed for the two, because the saturated solution of hydrophilic-basic swelling agent is inorganic solution, nonionic chelating agent is organic
More preferable mixing between the two may be implemented by ultrasonic power for solution.
In the present embodiment, the additive amount of the nonionic chelating agent is the saturated solution of the hydrophilic-basic swelling agent
The 1%-5% of mass fraction.
Specifically, in step s 30, expansion tears layer agent open and is sufficiently mixed the shape between the graphite linings of the oily phase graphite raw material
At oil mixture, mixed inorganic metal ion enters in the ligand of nonionic chelating agent, inorganic non-metallic ion shape
At free state, and penetrate into graphite between layers.
Specifically, in step s 40, it is one of EDTA, TDPA and EHDT or a variety of, institute that the chelating, which hits agent,
It states and chelates the 10% of the mass fraction that the additive amount for hitting agent is the oil mixture.The addition that chelating hits agent mainly obtains
The negative valency electronics in the inorganic non-metallic ion of free state is taken, to chelate nominal price inorganic metal ion, at this point, inorganic non-metallic
Ion is converted into carbon dioxide or oxygen, heat release in reaction process after losing electronics, to interrupt the model of graphite between layers
De Huali realizes the removing between graphite linings.
In another embodiment of the invention, a kind of application of the stripping means of graphene, the oil phase stone are also disclosed
Black alkene, which is added into automobile engine oil, plays lubricating action.
Embodiment one
A kind of stripping means of oily phase graphene of the present invention, calculates according to the mass fraction, includes the following steps:
1,3 parts of natural flake graphite powder and 6 parts of base oils are added in screw rod blender, and are stirred and form oil
Phase graphite raw material;
2, it is continuously added 1 part of expansion in whipping process and tears a layer agent open;
3,3h-5h is stirred, so that the expansion is torn layer agent open and is sufficiently mixed the shape between the graphite linings of the oily phase graphite raw material
At oil mixture;
4,1.1 parts of chelatings are hit in the agent addition oil mixture and stirs evenly to form oily phase reaction object;
5, the oily phase reaction object stands reaction 1-1.5h, forms the oily phase graphene.
The graphene surface of graphene prepared by the present invention shows fold pattern, and thickness is about 1~2nm, and length is about
0.5~5um.During the products application in the present embodiment to practical auto lubrication, in discharge detection, waste emission is reduced
50% or more, degree of lubrication improves 40%-75%, can achieve good energy saving, raising environment protecting.About this hair
The basic performance safety of the graphene of bright preparation, is suitable in investment actual production use process, detailed performance examining report is such as
Shown in attached drawing 2-7.
Disclosed above is only several specific embodiments of the invention, but the present invention is not limited to this, any ability
What the technical staff in domain can think variation should all fall into protection scope of the present invention.
Claims (10)
1. a kind of stripping means of oil phase graphene, which comprises the steps of:
Natural flake graphite powder is added in base oil and is stirred to form oily phase graphite raw material;
It is continuously added expansion in whipping process and tears a layer agent open;
3h-5h is stirred, so that the expansion is torn layer agent open and is sufficiently mixed the oily phase of formation between the graphite linings of the oily phase graphite raw material
Mixture;
Chelating is hit in the agent addition oil mixture and stirs evenly to form oily phase reaction object;
The oil phase reaction object stands reaction 1-1.5h, forms the oily phase graphene.
2. the stripping means of oil phase graphene according to claim 1, which is characterized in that the natural flake graphite powder
Having a size of -15000 mesh of 300 mesh.
3. the stripping means of oil phase graphene according to claim 2, which is characterized in that lubricated based on the base oil
Machine oil.
4. the stripping means of oil phase graphene according to claim 1, which is characterized in that the natural flake graphite powder with
The mixed proportion of base oil, is calculated based on mass fraction, natural flake graphite powder: base oil=1:2.
5. the stripping means of oil phase graphene according to claim 1, which is characterized in that the oil phase graphite raw material with it is swollen
The swollen mixed proportion for tearing layer agent open, is calculated based on mass fraction, oily phase graphite raw material: a layer agent=9:1 is torn in expansion open.
6. the stripping means of oil phase graphene according to claim 1, which is characterized in that described to expand the preparation for tearing layer agent open
Method includes the following steps:
By hydrophilic-basic swelling agent and water mixed dissolution, the saturated solution of the hydrophilic-basic swelling agent is formed;
The saturated solution of the hydrophilic-basic swelling agent is added in nonionic chelating agent, by ultrasonic agitation, forms emulsification
A layer agent is torn in the expansion of state open.
7. the stripping means of oil phase graphene according to claim 6, which is characterized in that the nonionic chelating agent adds
Dosage is the 1%-5% of the mass fraction of the saturated solution of the hydrophilic-basic swelling agent.
8. the stripping means of oil phase graphene according to claim 6, which is characterized in that the hydrophilic-basic swelling agent is
One of sodium bicarbonate, precipitated calcium carbonate and sodium peroxide are a variety of, the nonionic chelating agent be EDTA, TDPA and
One of EHDT or a variety of.
9. the stripping means of oil phase graphene according to claim 8, which is characterized in that the chelating hits agent and is
One of EDTA, TDPA and EHDT or a variety of, the additive amount that the chelating hits agent is the quality of the oil mixture
The 10% of score.
10. a kind of application based on the stripping means of mailbox graphene described in claim 1-9, which is characterized in that the oil
Phase graphene, which is added into automobile engine oil, plays lubricating action.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113735101A (en) * | 2021-09-23 | 2021-12-03 | 上海烯望新材料科技有限公司 | Method for preparing lipophilic few-layer graphene by stripping method |
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CN106966385A (en) * | 2016-10-13 | 2017-07-21 | 柯良节 | A kind of preparation method of graphene |
CN107267269A (en) * | 2017-07-19 | 2017-10-20 | 柯良节 | Feature graphene lubricating grease material and preparation method thereof |
CN107673335A (en) * | 2017-01-04 | 2018-02-09 | 柯良节 | Graphene preparation method based on the reaction of multiphase quantum self coupling |
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2019
- 2019-08-16 CN CN201910759684.6A patent/CN110371960A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US20110046027A1 (en) * | 2009-08-19 | 2011-02-24 | Aruna Zhamu | Nano graphene-modified lubricant |
CN106966385A (en) * | 2016-10-13 | 2017-07-21 | 柯良节 | A kind of preparation method of graphene |
CN107673335A (en) * | 2017-01-04 | 2018-02-09 | 柯良节 | Graphene preparation method based on the reaction of multiphase quantum self coupling |
CN107267269A (en) * | 2017-07-19 | 2017-10-20 | 柯良节 | Feature graphene lubricating grease material and preparation method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113735101A (en) * | 2021-09-23 | 2021-12-03 | 上海烯望新材料科技有限公司 | Method for preparing lipophilic few-layer graphene by stripping method |
CN113735101B (en) * | 2021-09-23 | 2024-04-09 | 上海烯望新材料科技有限公司 | Method for preparing lipophilic few-layer graphene by stripping method |
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