CN107487769A - A kind of method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid - Google Patents
A kind of method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid Download PDFInfo
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- CN107487769A CN107487769A CN201710658815.2A CN201710658815A CN107487769A CN 107487769 A CN107487769 A CN 107487769A CN 201710658815 A CN201710658815 A CN 201710658815A CN 107487769 A CN107487769 A CN 107487769A
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- Prior art keywords
- oil
- fluoride
- fluorinated graphene
- supercritical fluid
- prepared
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000012530 fluid Substances 0.000 title claims abstract description 28
- KRHYYFGTRYWZRS-UHFFFAOYSA-M fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 27
- 230000002687 intercalation Effects 0.000 claims abstract description 31
- 238000009830 intercalation Methods 0.000 claims abstract description 31
- 239000002199 base oil Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000000138 intercalating agent Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 11
- SFZCNBIFKDRMGX-UHFFFAOYSA-N Sulfur hexafluoride Chemical group FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 claims description 10
- 229960000909 sulfur hexafluoride Drugs 0.000 claims description 10
- -1 fluorine carbon Chemical compound 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 238000003682 fluorination reaction Methods 0.000 abstract description 13
- 239000010687 lubricating oil Substances 0.000 abstract description 11
- 239000010410 layer Substances 0.000 abstract description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 5
- 239000001569 carbon dioxide Substances 0.000 abstract description 5
- 239000011229 interlayer Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- YIOVLZNTAKLBQA-UHFFFAOYSA-M S(F)(F)(F)(F)(F)F.[F-] Chemical compound S(F)(F)(F)(F)(F)F.[F-] YIOVLZNTAKLBQA-UHFFFAOYSA-M 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 5
- 239000000523 sample Substances 0.000 description 4
- 238000007906 compression Methods 0.000 description 3
- 239000002826 coolant Substances 0.000 description 3
- 230000002349 favourable Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 230000003466 anti-cipated Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 231100000045 chemical toxicity Toxicity 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004808 supercritical fluid chromatography Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention belongs to functional material preparation field, more particularly, to a kind of method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid.Fluorographite is placed in autoclave, then is passed through intercalation remover fluoride sulfur hexafluoride, dispersant and auxiliary intercalator are lube base oil.Normal pressure is depressurized to after being circulated under postcritical pressure and temperature, is iteratively repeated said process.The disengaging fluorographite interlayer that fluoride intercalation remover quickly penetrates repeatedly, expanding and splitting fluorographite layer simultaneously, lube base oil enters fluorographite interlayer as auxiliary intercalation, finally it is made the oil-soluble fluorinated graphene material of two-dimensional nano thickness, the material proportion is close to commercial lubricating oil.Using fluoride supercritical fluid than the conventional supercritical fluid condition such as carbon dioxide milder safety, while the degree of fluorination of fluorinated graphene is ensured and strengthens, oily intercalation fluorinated graphene product is beneficial to disperse in lubricating oil.
Description
Technical field
It is molten using fluoride supercritical fluid preparation oil more particularly, to one kind the invention belongs to functional material preparation field
The method of property fluorinated graphene.
Background technology
Fluorinated graphene is high-tech, high-performance, the two-dimensional material of high benefit in the world now.Its performance is remarkable, quality
Uniqueness, it is a wonderful work in functional material family.With high temperature resistant, lubricity is high, and chemical stability is good, corrosion-resistant, dredges
Water oleophobic.Disclosed seldom by the document for preparing fluorinated graphene for synthesizing fluorographite, and difficulty is higher, and yield is few.Mostly
Using graphene as presoma, with fluorine gas or fluorination hydrofluorination, chemical toxicity is big, seriously polluted.Also useful ultrasound peels off fluorination stone
The method of ink, but yield efficiency is too low.
" method (publication number of preparation large scale fluorinated graphene is peeled off using supercritical carbon dioxide in Patents
CN105645398A although comparatively safe with carbon dioxide in) ", super critical condition is again too high, although carbon dioxide critical
Temperature is 31.26 DEG C, but critical pressure is high, is 7.3MPa.Moreover, fluorinated graphene degree of fluorination may in overcritical stripping process
Decline.
Meanwhile fluorinated graphene causes to be difficult to disperse in lubricating oil because its surface energy is extremely low and hydrophobic oleophobic.It is most of
The defluorinate of Chemical modification method in various degree is cost, sacrifices its important antifriction performance, causes its tribology to be anticipated
Extreme loss in justice.
The content of the invention
The defects of in order to overcome above-mentioned prior art to exist, face it is an object of the invention to provide one kind using fluoride is super
The method that boundary's fluid one-step method prepares oil-soluble fluorinated graphene, this method technique is simple, and degree of fluorination can be with stripping process
It is protected or improves.
The technical scheme is that：
A kind of method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, this method are inserted using overcritical
Layer stripping media be sulfur hexafluoride, dispersant and to aid in intercalator be lube base oil, is comprised the following steps and technique：
(1) fluorographite is added in autoclave, it is lube base oil to add dispersant and auxiliary intercalator；
(2) it is 0.1~10 by overcritical intercalation stripping media and fluorographite mass ratio:1, treat reaction under high pressure temperature in the kettle
After reaching default overcritical value with pressure, overcritical intercalation stripping media starts the cycle over flowing, treats overcritical intercalation stripping media
Circulate after the time reaches predetermined value, autoclave pressure is down to normal pressure；
(3) repeat above-mentioned (2) process, make material experience buck process repeatedly, by control boost and decompression number come
The graphene number of plies is controlled, that is, oil-soluble fluorinated graphene is prepared.
The described method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, in step (1), it is fluorinated stone
Ink is commercial fluorided graphite, and fluorine carbon mol ratio is 0.2~1.12.
The described method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, sulfur hexafluoride and lubricating oil
The mass ratio of base oil is 1:1~10.
The described method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, in step (2), high pressure is anti-
It is 46~100 DEG C to answer the temperature in kettle, and the pressure in autoclave is 4MPa~7MPa.
The described method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, it is overcritical in step (2)
Intercalation stripping media circulated the time as 1~60 minute, and the time for being deflated to normal pressure is 5~30 seconds.
The described method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, in step (3), boosting and
It is 1~10 time to be depressured number.
The present invention design philosophy be：
Fluorographite is placed in autoclave by the present invention, then is passed through intercalation remover fluoride sulfur hexafluoride, is disperseed
Agent and auxiliary intercalator are lube base oil.Normal pressure is depressurized to after being circulated under postcritical pressure and temperature, repeatedly
Repeat said process.The disengaging fluorographite interlayer that fluoride intercalation remover quickly penetrates repeatedly, in the fluorination that expands and split
Simultaneously, lube base oil enters fluorographite interlayer to graphite linings as auxiliary intercalation, and the oil of two-dimensional nano thickness is finally made
Dissolubility fluorinated graphene material, the material proportion is close to commercial lubricating oil.Carbon dioxide is compared using fluoride supercritical fluid
Deng conventional supercritical fluid condition milder safety, while ensure and strengthen the degree of fluorination of fluorinated graphene, oily intercalation fluorinated graphene
Product is beneficial to disperse in lubricating oil.
Compared with prior art, advantages of the present invention and beneficial effect are：
1st, the present invention utilizes sulfur hexafluoride at supercritical conditions, makes to be dispersed in the fluorographite stripping in lube base oil
From.Overcritical fluoride fluid permeability enters among the layer structure of fluorographite, reduces the effect of fluorographite between layers
Power.
2nd, while the present invention peels off fluorographite by overcritical fluoride, the fluorination of fluorographite is kept well
Degree, lube base oil do dispersant and aid in the fluorinated graphene proportion that intercalator to peel off more to hold close to base oil
Easily it is distributed in lubricating oil.
3rd, present invention process process is simple, and a step is completed, and condition is gentle safely, and product degree of fluorination is stable.
Brief description of the drawings
Fig. 1 is the apparatus structure schematic diagram for preparing fluorinated graphene；
In Fig. 1,1, SF 6 high-voltage bottle；2nd, pressure gauge；3rd, valve；4th, temperature probe；5th, agitator；6th, heater；
7th, surge tank；8th, compression pump；9th, coolant jacket；10th, autoclave；11st, lube base oil tank；12nd, reaction chamber.
Fig. 2 is the sample of fluorinated graphene.
Embodiment
In specific implementation process, the present invention prepares the side of oil-soluble fluorinated graphene using fluoride supercritical fluid
Method, this method use overcritical intercalation stripping media as sulfur hexafluoride, and dispersant and auxiliary intercalator are lube base oil, are adopted
Prepared with following steps and technique：
(1) fluorographite is added in autoclave, it is lube base oil to add dispersant and auxiliary intercalator；Fluorine
Graphite is commercial fluorided graphite, and fluorine carbon mol ratio is 0.2~1.12 (being preferably 0.6~1.1), sulfur hexafluoride and lubricating oil
Base oil mass ratio is 1:1~10 (is preferably 1:1.5~5.0).
(2) it is 0.1~10 by overcritical intercalation stripping media and fluorographite mass ratio:1 (is preferably 2~5:1), it is pumped into
In autoclave, after temperature and pressure in autoclave reaches default overcritical value, overcritical intercalation stripping media is opened
Beginning circulates, and is circulated after overcritical intercalation stripping media after the time reaches predetermined value, is down to autoclave pressure
Normal pressure；Temperature in autoclave is 46~100 DEG C, and the pressure in autoclave (is preferably, temperature for 4MPa~7MPa
For 46~60 DEG C, 4~5MPa of pressure).Overcritical intercalation stripping media circulated the time as 1~60 minute, was deflated to normal pressure
Time for 5~30 seconds (be preferably, temperature be 30~60 minutes, venting duration 5~15 seconds).
(3) above-mentioned (2) process is repeated, makes material experience buck process repeatedly, number (1 is boosted and be depressured by controlling
~10 times) control the graphene number of plies, that is, it is prepared oil-soluble fluorinated graphene.In oil-soluble fluorinated graphene, less than 10
The fluorinated graphene of layer accounts for 80wt%, and degree of fluorination (i.e. fluorine carbon mol ratio) is 1.0.
As shown in figure 1, the present invention prepares the device of oil-soluble fluorinated graphene, mainly include：SF 6 high-voltage bottle 1,
Pressure gauge 2, valve 3, temperature probe 4, agitator 5, heater 6, surge tank 7, compression pump 8, coolant jacket 9, autoclave 10,
Lube base oil 11, reaction chamber 12, concrete structure is as follows：
Reaction chamber 12 is set in autoclave 10, and the outside of reaction chamber 12 sets coolant jacket 9, heating is set in reaction chamber 12
Device 6, the stirring end of agitator 5 extend reaction chamber 12, and the thermometric end of temperature probe 4 extends reaction chamber 12；SF 6 high-voltage bottle 1
Connected by pipeline with reaction chamber 12, pressure gauge 2, valve 3 are set on the pipeline；One end of surge tank 7 is connected to by pipeline
Reaction chamber 12, valve 3 is set on the pipeline；The output that the other end of surge tank 7 passes through pipeline and lube base oil tank 11
Pipeline converges, and compression pump 8 is set on the output pipe of the surge tank 7, can circulate and be pumped into autoclave.
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
In the present embodiment, method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, use is overcritical
SF6For remover, in the case that lube base oil is dispersant and auxiliary intercalator, comprise the following steps：
It is 1.0 10 grams of fluorographite and overcritical 20 grams of fluids of intercalation stripping media sulfur hexafluoride by fluorine carbon ratio, lubricates
60 grams of oil base oil, is pumped into autoclave；Treat that temperature and pressure reaches 50 DEG C in autoclave, 6MPa presets overcritical
After value, overcritical intercalation stripping media starts the cycle over flowing, after overcritical intercalation stripping media circulates 1 hour time,
Pressure release makes pressure in kettle be down to normal pressure to surge tank in 6 seconds；Said process is repeated, makes material experience buck process 6 repeatedly
It is secondary, oil-soluble fluorinated graphene (Fig. 2) is prepared.
Characterized by testing, the fluorinated graphene in product less than 10 layers accounts for 70wt%, product degree of fluorination 1.0, lubricating oil
In favorable dispersibility.
Embodiment 2
In the present embodiment, method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, use is overcritical
SF6For main remover, the use of lube base oil is dispersant and auxiliary intercalator, comprises the following steps：
It is 1.1 10 grams of fluorographite and overcritical 20 grams of fluids of intercalation stripping media sulfur hexafluoride by fluorine carbon ratio, lubricates
50 grams of oil base oil, is pumped into autoclave；Treat that temperature and pressure reaches 46 DEG C in autoclave, 6MPa presets overcritical
After value, overcritical intercalation stripping media starts the cycle over flowing, after overcritical intercalation stripping media circulates 1 hour time,
Pressure release makes pressure in kettle be down to normal pressure to surge tank in 8 seconds；Said process is repeated, makes material experience buck process 8 repeatedly
It is secondary, oil-soluble fluorinated graphene is prepared.
Characterized by testing, the fluorinated graphene in product less than 10 layers accounts for 75wt%, product degree of fluorination 1.1, lubricating oil
In favorable dispersibility.
Embodiment 3
In the present embodiment, method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, use is overcritical
SF6For main remover, the use of lube base oil is dispersant and auxiliary intercalator, comprises the following steps：
It is 0.75 10 grams of fluorographite and overcritical 25 grams of fluids of intercalation stripping media sulfur hexafluoride by fluorine carbon ratio, lubricates
40 grams of oil base oil, is pumped into autoclave；Treat that temperature and pressure reaches 55 DEG C in autoclave, 6.0MPa presets super face
After dividing value, overcritical intercalation stripping media starts the cycle over flowing, treats that overcritical intercalation stripping media circulates the time 0.5 hour
Afterwards, pressure release makes pressure in kettle be down to normal pressure to surge tank in 10 seconds；Said process is repeated, making material experience, lifting presses through repeatedly
Journey 8 times, is prepared oil-soluble fluorinated graphene.
Characterized by testing, the fluorinated graphene in product less than 10 layers accounts for 80wt%, product degree of fluorination 0.75, lubricating oil
In favorable dispersibility.
Claims (6)
- A kind of 1. method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, it is characterised in that this method is adopted It is sulfur hexafluoride with overcritical intercalation stripping media, dispersant and auxiliary intercalator are lube base oil, are comprised the following steps And technique：(1) fluorographite is added in autoclave, it is lube base oil to add dispersant and auxiliary intercalator；(2) it is 0.1~10 by overcritical intercalation stripping media and fluorographite mass ratio:1, treat reaction under high pressure temperature in the kettle and pressure After power reaches default overcritical value, overcritical intercalation stripping media starts the cycle over flowing, treats overcritical intercalation stripping media circulation After flowing time reaches predetermined value, autoclave pressure is set to be down to normal pressure；(3) above-mentioned (2) process is repeated, makes material experience buck process repeatedly, number is boosted and be depressured to control by controlling The graphene number of plies, that is, oil-soluble fluorinated graphene is prepared.
- 2. the method according to claim 1 that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, it is special Sign is, in step (1), fluorographite is commercial fluorided graphite, and fluorine carbon mol ratio is 0.2~1.12.
- 3. the method according to claim 1 that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, it is special Sign is that the mass ratio of sulfur hexafluoride and lube base oil is 1:1~10.
- 4. the method according to claim 1 that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, it is special Sign is, in step (2), temperature in autoclave is 46~100 DEG C, the pressure in autoclave for 4MPa~ 7MPa。
- 5. the method according to claim 1 that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, it is special Sign is, in step (2), overcritical intercalation stripping media circulated the time as 1~60 minute, and the time for being deflated to normal pressure is 5~30 seconds.
- 6. the method according to claim 1 that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid, it is special Sign is, in step (3), boosting and decompression number are 1~10 time.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710658815.2A CN107487769A (en) | 2017-08-04 | 2017-08-04 | A kind of method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid |
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| CN201710658815.2A CN107487769A (en) | 2017-08-04 | 2017-08-04 | A kind of method that oil-soluble fluorinated graphene is prepared using fluoride supercritical fluid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111232982A (en) * | 2020-03-18 | 2020-06-05 | 中国科学院宁波材料技术与工程研究所 | Two-dimensional Ti3C2TXMethod for peeling nanosheet |
| CN112624098A (en) * | 2021-01-20 | 2021-04-09 | 湖北卓熙氟化股份有限公司 | Preparation method and application of fluorinated graphene with high fluorocarbon ratio |
| CN113772666A (en) * | 2021-10-25 | 2021-12-10 | 大连元晶科技有限公司 | Method for preparing oil-soluble fluorinated graphene by stripping with supercritical carbon dioxide |
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| CN111232982A (en) * | 2020-03-18 | 2020-06-05 | 中国科学院宁波材料技术与工程研究所 | Two-dimensional Ti3C2TXMethod for peeling nanosheet |
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| CN113772666A (en) * | 2021-10-25 | 2021-12-10 | 大连元晶科技有限公司 | Method for preparing oil-soluble fluorinated graphene by stripping with supercritical carbon dioxide |
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Application publication date: 20171219 |