CN106167262A - A kind of utilize graphene oxide to the method increasing oil lubrication and heat conductivity - Google Patents
A kind of utilize graphene oxide to the method increasing oil lubrication and heat conductivity Download PDFInfo
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- CN106167262A CN106167262A CN201610532693.8A CN201610532693A CN106167262A CN 106167262 A CN106167262 A CN 106167262A CN 201610532693 A CN201610532693 A CN 201610532693A CN 106167262 A CN106167262 A CN 106167262A
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- deionized water
- graphene oxide
- heat conductivity
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- oil lubrication
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to a kind of utilize graphene oxide to the method increasing oil lubrication and heat conductivity, comprise the following steps: 1) Potassium hyposulfite., phosphorus pentoxide and concentrated sulphuric acid are sequentially added in flask, dissolve at 80 DEG C, add graphite powder, stir at 80 DEG C, after question response terminates, add deionized water, finally carry out repeatedly sucking filtration with deionized water, then be dried at 50 DEG C；2) pre-oxidation product is joined in concentrated sulphuric acid, under ice bath, be slowly added to potassium permanganate, react at 35 DEG C afterwards, be slow added into deionized water, finally pour in flask, add deionized water and hydrogen peroxide；3) by product chlorohydric acid pickling, then dialyse in deionized water with bag filter；4) by graphene oxide, ethanol and 18-amine. hybrid reaction, clean with ethanol sucking filtration, the most i.e. obtain end product；Present invention improves lubricity and the heat conductivity of lubricating oil, whole process operation is simple, safety, and effective.
Description
[technical field]
The invention belongs to chemical technology field, specifically one utilizes graphene oxide to increase oil lubrication
Method with heat conductivity.
[background technology]
Graphene be a kind of monoatomic layer that last decade grows up be the transparent material of two-dimensional network structure, its conduction
Property, heat conductivity, light transmission good, mechanical strength is better than existing other materials, by the pre-optimal material for making high ladder.From 2004
Year first since experiment obtains graphene sheet layer, its application in terms of biology, medical science, photoelectric material, quasiconductor and conductor
Obtain unprecedented development, owing to Graphene also exists the performance of excellence, be therefore that 21 century is most important newly in advance by people
Shaped material.At present, the method preparing Graphene has mechanical stripping method, vapour deposition process, epitaxial growth method and oxidation-reduction method.?
In these methods, oxidation-reduction method has preparation process is simple and production cost is low advantage it is considered to be best suitable for industrialization
The method produced.The existing oxidation-reduction method preparing Graphene mainly include Hummers method, Brodie method and
Standenmaier method.Now according to the difference of Graphene application, the method for modifying taking it is also not quite similar, mainly
There is covalent bond to modify and non-covalent bond is modified.
At present, lubricating oil lubricity and heat conductivity in special application still can not meet demand, particularly heat conductivity
With fretting wear aspect, therefore according to concrete application, improve the performance of this two aspect of lubricating oil, have become as a kind of demand.
[summary of the invention]
Present invention aim to solve above-mentioned deficiency and provide one to utilize graphene oxide to increase lubricating oil
Lubricity and the method for heat conductivity, utilize lubricity and the heat conductivity of lubricity and the improved thermal conductivity lubricating oil of Graphene,
Whole process operation is simple, safety, and effective.
Design for achieving the above object a kind of utilize graphene oxide to the method increasing oil lubrication and heat conductivity,
Comprise the following steps,
1) step that graphite powder is pre-oxidized: Potassium hyposulfite., phosphorus pentoxide and concentrated sulphuric acid are sequentially added in flask,
Dissolve at 80 DEG C, be subsequently adding graphite powder, at 80 DEG C, stir 4.5h, after question response terminates, add deionized water, finally use
Deionized water carries out repeatedly sucking filtration, then is dried 24h at 50 DEG C；
2) by the step of product reoxidation after pre-oxidation: by step 1) the pre-oxidation product of gained joins concentrated sulphuric acid
In, under ice bath, it is slowly added to potassium permanganate, at 35 DEG C, reacts 2h afterwards, be slow added into deionized water, finally pour burning into
In Ping, add deionized water and hydrogen peroxide；
3) by the product pickling after oxidation, the step of dialysis: by step 2) product of gained carries out acid with the hydrochloric acid of 10%
Wash one week, then dialyse in deionized water with bag filter 10 days, the most just obtained graphite oxide ene product；
4) graphene oxide is carried out the process of 18-amine. modification: graphene oxide, ethanol and 18-amine. are mixed, instead
Should, the product ethanol sucking filtration obtained cleans, and the most i.e. obtains end product.
As preferably, step 1) in, described graphite powder be mesh number be the graphite powder of 5000.
As preferably, step 1) and step 2) in, the mass percent concentration of described concentrated sulphuric acid is 98%.
As preferably, step 2) in, described hydrogen peroxide is the hydrogen peroxide of 30% concentration.
As preferably, step 4) in, when modifying 18-amine., first 18-amine. is dissolved in ethanol, then it is slowly added
Enter in graphene oxide solution, addition limit, limit magnetic agitation.
As preferably, step 4) in, the modification time of described 18-amine. is 20 hours, and reaction temperature is 90 DEG C, reacts
Adding a reflux in journey, reflux is used for preventing ethanol and deionized water in solution from reducing.
As preferably, step 1) and step 2) in, the step adding deionized water is: first, when room temperature is less than 15 DEG C
Directly being positioned in air by flask, stirring, while being slowly added to deionized water, temperature is 40-50 DEG C, works as deionized water
After having added half, being put into by flask in 40 DEG C of oil cauldrons, then continue to add deionized water, temperature is still 40-50 DEG C.
The present invention compared with the existing technology, with graphite powder as raw material, prepares graphene oxide with Hummers improved method,
Employing covalent bond is modified, the way with 18-amine. as dressing agent, and its advantage is to allow the graphene oxide insoluble in oil good
It is dissolved in various lubricating oil, thus improves lubricity and the heat conductivity of lubricating oil, i.e. feature chemical modification of the present invention
Graphene oxide is dissolved in lubricating oil by method, then utilizes lubricity and the lubrication of improved thermal conductivity lubricating oil of Graphene
Property and heat conductivity, its technological progress is significant, and whole experimentation is simple to operate, safety, and effective, be worthy to be popularized should
With.
[detailed description of the invention]
The invention provides a kind of utilize graphene oxide to the method increasing oil lubrication and heat conductivity, including one
The individual step that graphite powder is pre-oxidized；One step to pre-oxidation product sucking filtration, is carried out the product after sucking filtration at 50 DEG C
Baking；One carries out the step of reoxidation to dried product after pre-oxidation, with potassium permanganate and concentrated sulphuric acid as oxidant,
Use Hummers method to aoxidize, pre-oxidation product is aoxidized under the conditions of concentrated sulphuric acid and potassium permanganate；One to oxidation
Product carries out the process of pickling and dialysis, is cleaned with the hydrochloric acid of 10% by the oxidation product obtained, after finally being cleaned by hydrochloric acid
Product deionized water is dialysed, and finally obtains the graphite oxide ene product of liquid；One carries out 18 to graphene oxide
Amine-modified process, mixes graphene oxide, ethanol and 18-amine., and 90 DEG C of reactions, the product ethanol sucking filtration obtained is clear
Wash, the most just obtain end product.Wherein, the mass percent concentration of concentrated sulfuric acid solution is 98%, and hydrogen peroxide is 30% dense
The hydrogen peroxide of degree.
Specifically, the step added water in graphite powder oxidizing process is: first, when room temperature is less than 15 DEG C directly by flask
Being positioned in air, stirring, while being slowly added to water, temperature is not higher than 50 DEG C but not below 40 DEG C yet.When water adds
After half, being put into by flask in 40 DEG C of oil cauldrons, then continue to add water, temperature still do not exceeds 50 DEG C, and the most not below 40
℃.The condition that graphene oxide is modified is: is first dissolved in ethanol by 18-amine. during reaction, is slowly added into oxidation the most again
In graphene solution, addition limit, limit magnetic agitation, reaction temperature is 90 DEG C, and the response time is 20 hours, adds one in course of reaction
Individual reflux, prevents ethanol and deionized water in solution from reducing.
The present invention utilize graphene oxide to increase oil lubrication and heat conductivity, existing lubricating oil various specifically
Application in lubricity and heat conductivity still can not meet requirement, easily cause surface between phase mutual friction workpiece and exist the biggest
Abrasion.The method increasing oil lubrication and heat conductivity has a lot, such as adds the little granule of various nanometer, but owing to these are received
The attribute of rice little granule itself, improvement degree still can not meet requirement.Graphene makes it certainly due to the structure of himself uniqueness
Body has good lubricity and heat conductivity, improves oil lubrication hence with Graphene and heat conductivity is one and is worth
The new method attempted.The method that the graphene oxide modified with 18-amine. improves oil lubrication and heat conductivity, its advantage is
Simple to operate, safety, and effective.
The present invention is made further explained below below in conjunction with specific embodiment:
Embodiment 1
(1) pre-oxidation of graphite powder
Potassium hyposulfite. (8.4g), phosphorus pentoxide (8.4g) and concentrated sulphuric acid (50ml) are sequentially added in flask at 80 DEG C
Lower dissolving.Be subsequently adding 10g pre-oxidize graphite powder, graphite powder be mesh number be the graphite powder of 5000, at 80 DEG C stir 4.5h, etc.
Reaction adds deionized water (100ml) after terminating, finally carry out repeatedly sucking filtration with deionized water (1.6l), be finally dried at 50 DEG C
24h。
(2) reoxidation of the product after pre-oxidation
2g is pre-oxidized product and joins in 46ml concentrated sulphuric acid, under ice bath, be slowly added to 6g potassium permanganate, afterwards 35
At DEG C react 2h, be slowly added to 92ml deionized water afterwards, finally pour in baked cake add 280ml deionized water and
7.5ml hydrogen peroxide.
(3) pickling of the product after oxidation, dialysis
The product obtained is carried out pickling one week with the hydrochloric acid of 10%, then dialyses in deionized water with bag filter 10 days,
The most just oxidation product has been obtained.
(4) 18-amine. is modified in surface of graphene oxide
0.6g graphene oxide is dissolved in 300ml deionized water, and 0.6 18-amine. is dissolved in 90ml ethanol, finally by it
Slowly mix, and 90 DEG C react 20 hours, add a reflux during reaction.The product ethanol sucking filtration obtained is clear
Wash, the most just obtain end product.
Embodiment 2
(1) pre-oxidation of graphite powder
Potassium hyposulfite. (8.4g), phosphorus pentoxide (8.4g) and concentrated sulphuric acid (50ml) are sequentially added in flask at 80 DEG C
Lower dissolving.It is subsequently adding 10g and pre-oxidizes graphite powder, at 80 DEG C, stir 4.5h, after waiting reaction to terminate, add deionized water
(100ml), finally repeatedly sucking filtration is carried out, finally at 50 DEG C of dry 24h with deionized water (1.6l).
(2) reoxidation of the product after pre-oxidation
2g is pre-oxidized product and joins in 46ml concentrated sulphuric acid, under ice bath, be slowly added to 6g potassium permanganate, afterwards 35
At DEG C react 2h, be slowly added to 92ml deionized water afterwards, finally pour in baked cake add 280ml deionized water and
7.5ml hydrogen peroxide.
(3) pickling of the product after oxidation, dialysis
The product obtained is carried out pickling one week with the hydrochloric acid of 10%, then dialyses in deionized water with bag filter 10 days,
The most just oxidation product has been obtained.
(4) 18-amine. is modified in surface of graphene oxide
0.6g graphene oxide is dissolved in 300ml deionized water, and 0.9 18-amine. is dissolved in 90ml ethanol, finally by it
Slowly mix, and 90 DEG C react 20 hours, add a reflux during reaction.The product ethanol sucking filtration obtained is clear
Wash, the most just obtain end product.
Embodiment 3
(1) pre-oxidation of graphite powder
Potassium hyposulfite. (8.4g), phosphorus pentoxide (8.4g) and concentrated sulphuric acid (50ml) are sequentially added in flask at 80 DEG C
Lower dissolving.It is subsequently adding 10g and pre-oxidizes graphite powder, at 80 DEG C, stir 4.5h, after waiting reaction to terminate, add deionized water
(100ml), finally repeatedly sucking filtration is carried out, finally at 50 DEG C of dry 24h with deionized water (1.6l).
(2) reoxidation of the product after pre-oxidation
2g is pre-oxidized product and joins in 46ml concentrated sulphuric acid, under ice bath, be slowly added to 6g potassium permanganate, afterwards 35
At DEG C react 2h, be slowly added to 92ml deionized water afterwards, finally pour in baked cake add 280ml deionized water and
7.5ml hydrogen peroxide.
(3) pickling of the product after oxidation, dialysis
The product obtained is carried out pickling one week with the hydrochloric acid of 10%, then dialyses in deionized water with bag filter 10 days,
The most just oxidation product has been obtained.
(4) 18-amine. is modified in surface of graphene oxide
0.6g graphene oxide is dissolved in 300ml deionized water, and 1.2 18-amine. are dissolved in 120ml ethanol, finally by it
Slowly mix, and 90 DEG C react 20 hours, add a reflux during reaction.The product ethanol sucking filtration obtained is clear
Wash, the most just obtain end product.
The present invention is not limited by above-mentioned embodiment, other any spirit without departing from the present invention and principle
Lower made change, modify, substitute, combine, simplify, all should be the substitute mode of equivalence, be included in the protection model of the present invention
Within enclosing.
Claims (7)
1. one kind utilizes graphene oxide to the method increasing oil lubrication and heat conductivity, it is characterised in that include following
Step,
1) step that graphite powder is pre-oxidized: Potassium hyposulfite., phosphorus pentoxide and concentrated sulphuric acid are sequentially added in flask, 80
At DEG C dissolve, be subsequently adding graphite powder, at 80 DEG C stir 4.5h, after question response terminates, add deionized water, finally spend from
Sub-water carries out repeatedly sucking filtration, then is dried 24h at 50 DEG C；
2) by the step of product reoxidation after pre-oxidation: by step 1) the pre-oxidation product of gained joins in concentrated sulphuric acid,
Under ice bath, it is slowly added to potassium permanganate, at 35 DEG C, reacts 2h afterwards, be slow added into deionized water, finally pour flask into
In, add deionized water and hydrogen peroxide；
3) by the product pickling after oxidation, the step of dialysis: by step 2) product of gained carries out pickling one with the hydrochloric acid of 10%
Week, then dialyse in deionized water with bag filter 10 days, the most just obtain graphite oxide ene product；
4) graphene oxide is carried out the process of 18-amine. modification: graphene oxide, ethanol and 18-amine. are mixed, reaction,
The product ethanol sucking filtration arrived cleans, and the most i.e. obtains end product.
Utilize the most as claimed in claim 1 graphene oxide to the method increasing oil lubrication and heat conductivity, its feature
Be: step 1) in, described graphite powder be mesh number be the graphite powder of 5000.
Utilize the most as claimed in claim 1 graphene oxide to the method increasing oil lubrication and heat conductivity, its feature
It is: step 1) and step 2) in, the mass percent concentration of described concentrated sulphuric acid is 98%.
Utilize the most as claimed in claim 1 graphene oxide to the method increasing oil lubrication and heat conductivity, its feature
It is: step 2) in, described hydrogen peroxide is the hydrogen peroxide of 30% concentration.
Utilize the most as claimed in claim 1 graphene oxide to the method increasing oil lubrication and heat conductivity, its feature
It is: step 4) in, when modifying 18-amine., first 18-amine. is dissolved in ethanol, is then slowly added into graphite oxide
In alkene solution, addition limit, limit magnetic agitation.
Utilize the most as claimed in claim 1 graphene oxide to the method increasing oil lubrication and heat conductivity, its feature
It is: step 4) in, the modification time of described 18-amine. is 20 hours, and reaction temperature is 90 DEG C, adds one and return in course of reaction
Stream device, reflux is used for preventing ethanol and deionized water in solution from reducing.
Utilize the most as claimed in claim 1 graphene oxide to the method increasing oil lubrication and heat conductivity, its feature
It is: step 1) and step 2) in, the step adding deionized water is: first, is directly put by flask when room temperature is less than 15 DEG C
Being placed in air, stirring, while being slowly added to deionized water, temperature is 40-50 DEG C, after deionized water has added half,
Being put into by flask in 40 DEG C of oil cauldrons, then continue to add deionized water, temperature is still 40-50 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107523004A (en) * | 2017-09-11 | 2017-12-29 | 中山大学 | A kind of high barrier material of macromolecule intercalation graphene oxide and preparation method thereof |
| CN107686762A (en) * | 2017-09-18 | 2018-02-13 | 吴江华威特种油有限公司 | A kind of resistance to oxidation heat-conducting type lubricating oil and preparation method thereof |
| CN109097168A (en) * | 2018-08-31 | 2018-12-28 | 郑州市欧普士科技有限公司 | A kind of nano-graphene constant velocity cardan joint special grease and preparation method thereof |
| CN114437858A (en) * | 2022-02-09 | 2022-05-06 | 沈阳建筑大学 | Graphene oxide lubricating oil and preparation method thereof |
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| CN104616826A (en) * | 2014-12-30 | 2015-05-13 | 浙江大学 | Graphene-PDMS (Polydimethylsiloxane) flexible electrode and preparation method and application thereof |
| CN104725729A (en) * | 2013-12-24 | 2015-06-24 | 中国科学院宁波材料技术与工程研究所 | Ethylene propylene diene monomer rubber/polypropylene composite material and preparation thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104725729A (en) * | 2013-12-24 | 2015-06-24 | 中国科学院宁波材料技术与工程研究所 | Ethylene propylene diene monomer rubber/polypropylene composite material and preparation thereof |
| CN104616826A (en) * | 2014-12-30 | 2015-05-13 | 浙江大学 | Graphene-PDMS (Polydimethylsiloxane) flexible electrode and preparation method and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107523004A (en) * | 2017-09-11 | 2017-12-29 | 中山大学 | A kind of high barrier material of macromolecule intercalation graphene oxide and preparation method thereof |
| CN107686762A (en) * | 2017-09-18 | 2018-02-13 | 吴江华威特种油有限公司 | A kind of resistance to oxidation heat-conducting type lubricating oil and preparation method thereof |
| CN109097168A (en) * | 2018-08-31 | 2018-12-28 | 郑州市欧普士科技有限公司 | A kind of nano-graphene constant velocity cardan joint special grease and preparation method thereof |
| CN114437858A (en) * | 2022-02-09 | 2022-05-06 | 沈阳建筑大学 | Graphene oxide lubricating oil and preparation method thereof |
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Application publication date: 20161130 |