CN101486456A - Industrial novel method for synthesizing fluorizated petroleum coke - Google Patents
Industrial novel method for synthesizing fluorizated petroleum coke Download PDFInfo
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- CN101486456A CN101486456A CNA2008100327874A CN200810032787A CN101486456A CN 101486456 A CN101486456 A CN 101486456A CN A2008100327874 A CNA2008100327874 A CN A2008100327874A CN 200810032787 A CN200810032787 A CN 200810032787A CN 101486456 A CN101486456 A CN 101486456A
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- fluorizated
- petroleum coke
- fluorine gas
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- reactor
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention discloses an industrial synthesis method of petroleum coke fluoride. Fluorine gas or the mixture of fluorine gas and inert gas is led into a certain reaction container at certain flow speed and pressure for reaction; and then petroleum coke fluoride of various specifications and with the fluorine content of more than 58 percent is obtained at certain temperature. Compared with method specified in other relevant patents, the method has simple operation and can fulfill industrial scale. The petroleum coke fluoride products obtained are mainly applied to the electrode materials of a novel high energy lithium ion battery.
Description
Technical field
Fluorizated petroleum coke is the solid lubricant with good lubricity, is widely used in fields such as national defence, machinery, precision instrument.
Background technology
The fluorizated petroleum coke synthetic method is a lot, and relevant patent report is all arranged both at home and abroad.With the synthetic fluorizated petroleum coke of diverse ways characteristics are arranged respectively.Synthetic fluorine content can reach more than 58% in the common laboratory, but fluorizated petroleum coke output is very low, can only small-scalely prepare.Under the prerequisite that general industry synthetic method turnout improves, fluorine content is difficult to improve, thereby the poor quality of fluorizated petroleum coke.
Summary of the invention
The invention provides a kind of industrial preparative method of fluorizated petroleum coke, this method is by control certain reaction condition, can plant-scale production fluorizated petroleum coke, and uniform in quality, fluorine content is more than 58%.
The described a kind of raw material of this patent is a refinery coke, and granularity is 0.01 micron to 500 microns.Another kind of raw material is a fluorine gas, perhaps passes through the fluorine gas behind the inert gas dilution, and the two reacts in reactor at a certain temperature, obtains fluorizated petroleum coke.
Preparing the described fluorizated petroleum coke of this patent carries out according to following steps: one, add refinery coke in reactor, vacuumize; Two, system is heated to specific temperature of reaction; Three, feed the mixed gas of fluorine gas or fluorine gas and rare gas element, fluorine gas and refinery coke generate fluorizated petroleum coke in reaction vessel, and unnecessary fluorine gas absorbs by the absorption tower that soda-lime and charcoal are housed; Four, treat temperature cooling after, open reactor, the fluorizated petroleum coke in the reactor is taken out.
Following example has been set forth the preparation method of fluorizated petroleum coke among the present invention:
Example one
Refinery coke is joined in the reaction vessel for 500 microns 600 kilograms, reactor is heated to 200 to 300 degree, vacuumize the reaction system air is caught up with only, twice repeatedly, temperature of reaction kettle is elevated to 300 to 500 degree, slowly feed fluorine gas, the flow velocity that adds fluorine gas by the control of fluorine gas flow meter is 3 to 50 liters of per minutes, under this flow, continue reaction 5 to 10 hours, stop heating, allow reactor naturally cool to the following temperature of 300 degree, feeding nitrogen in the refrigerative reaction vessel, drive fluorine gas remaining in the reactor away, reaction finishes.Open reactor, the solid powder in the reactor is pressed color classification take out, promptly get product, 1000 kilograms of product gross weights.
Example two
Refinery coke is joined in the reaction vessel for 50 microns 600 kilograms, reactor is heated to 200 to 300 degree, vacuumize the reaction system air is caught up with only, twice repeatedly, temperature of reaction kettle is elevated to 300 to 500 degree, slowly feed fluorine gas, the flow velocity that adds fluorine gas by the control of fluorine gas flow meter is 3 to 50 liters of per minutes, under this flow, continue reaction 5 to 10 hours, stop heating, allow reactor naturally cool to the following temperature of 300 degree, feeding nitrogen in the refrigerative reaction vessel, drive fluorine gas remaining in the reactor away, reaction finishes.Open reactor, the solid powder in the reactor is taken out, promptly get product, 1000 kilograms of product gross weights.
Example three
Refinery coke is joined in the reaction vessel for 10 microns 600 kilograms, reactor is heated to 200 to 300 degree, vacuumize the reaction system air is caught up with only, twice repeatedly, temperature of reaction kettle is elevated to 300 to 500 degree, slowly feed fluorine gas, the flow velocity that adds fluorine gas by the control of fluorine gas flow meter is 3 to 50 liters of per minutes, under this flow, continue reaction 5 to 10 hours, stop heating, allow reactor naturally cool to the following temperature of 300 degree, feeding nitrogen in the refrigerative reaction vessel, drive fluorine gas remaining in the reactor away, reaction finishes.Open reactor, the solid powder in the reactor is taken out, promptly get product, 1000 kilograms of product gross weights
Example four
Refinery coke is joined in the reaction vessel for 5 microns 600 kilograms, reactor is heated to 200 to 300 degree, vacuumize the reaction system air is caught up with only, twice repeatedly, temperature of reaction kettle is elevated to 300 to 500 degree, slowly feed fluorine gas, the flow velocity that adds fluorine gas by the control of fluorine gas flow meter is 3 to 50 liters of per minutes, under this flow, continue reaction 5 to 10 hours, stop heating, allow reactor naturally cool to the following temperature of 300 degree, feeding nitrogen in the refrigerative reaction vessel, drive fluorine gas remaining in the reactor away, reaction finishes.Open reactor, the solid powder in the reactor is taken out, promptly get product, 1000 kilograms of product gross weights
Example five
Refinery coke is joined in the reaction vessel for 1 micron 600 kilograms, reactor is heated to 200 to 300 degree, vacuumize the reaction system air is caught up with only, twice repeatedly, temperature of reaction kettle is elevated to 300 to 500 degree, slowly feed fluorine gas, the flow velocity that adds fluorine gas by the control of fluorine gas flow meter is 3 to 50 liters of per minutes, under this flow, continue reaction 5 to 10 hours, stop heating, allow reactor naturally cool to the following temperature of 300 degree, feeding nitrogen in the refrigerative reaction vessel, drive fluorine gas remaining in the reactor away, reaction finishes.Open reactor, the solid powder in the reactor is taken out, promptly get product, 1000 kilograms of product gross weights
Example six
Refinery coke is joined in the reaction vessel for 5 microns 600 kilograms, reactor is heated to 200 to 300 degree, vacuumize the reaction system air is caught up with only, twice repeatedly, temperature of reaction kettle is elevated to 300 to 500 degree, slowly feed fluorine gas and nitrogen mixture body (1:1), the flow velocity that adds gas mixture by the control of fluorine gas flow meter is 3 to 50 liters of per minutes, under this flow, continue reaction 5 to 10 hours, stop heating, allow reactor naturally cool to the following temperature of 300 degree, feeding nitrogen in the refrigerative reaction vessel, drive fluorine gas remaining in the reactor away, reaction finishes.Open reactor, the solid powder in the reactor is pressed color classification take out, promptly get product, 1000 kilograms of product gross weights
Example seven
Refinery coke is joined in the reaction vessel for 1 micron 600 kilograms, reactor is heated to 200 to 300 degree, vacuumize the reaction system air is caught up with only, twice repeatedly, temperature of reaction kettle is elevated to 300 to 500 degree, slowly feed the mixed gas of fluorine gas and nitrogen, the flow velocity that adds gas mixture by the control of fluorine gas flow meter is 3 to 50 liters of per minutes, under this flow, continue reaction 5 to 10 hours, stop heating, allow reactor naturally cool to the following temperature of 300 degree, feeding nitrogen in the refrigerative reaction vessel, drive fluorine gas remaining in the reactor away, reaction finishes.Open reactor, the solid powder in the reactor is taken out, promptly get product, 1000 kilograms of product gross weights.
Claims (1)
- The invention describes a kind of industrial preparative method of fluorizated petroleum coke.Carbon raw material is a refinery coke; Another raw material can be a fluorine gas, the mixed gas of fluorine gas and nitrogen or fluorine gas and argon gas; The two reacts at a certain temperature and obtains fluorizated petroleum coke, and product fluorine content is more than 58%.This method synthetic fluorizated petroleum coke product mainly is used as the electrode materials of a class novel high-energy lithium ion battery.The fluorizated petroleum coke that 1 reaction generates, it forms general formula can use (CF x) nExpression.0<x<1The carbon raw material of 2 these compounds of preparation is fluorizated petroleum cokes, and granular size is from 0.01 micron to 500 microns.3 reaction pressures are controlled at 1 to 10 normal atmosphere.4 temperature of reaction are controlled at 300 to 500 degrees centigrade of scope internal reactions.5 gas flows are controlled at 1 to 50 liter/minute.
Priority Applications (1)
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CNA2008100327874A CN101486456A (en) | 2008-01-17 | 2008-01-17 | Industrial novel method for synthesizing fluorizated petroleum coke |
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CNA2008100327874A CN101486456A (en) | 2008-01-17 | 2008-01-17 | Industrial novel method for synthesizing fluorizated petroleum coke |
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CN101486456A true CN101486456A (en) | 2009-07-22 |
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CNA2008100327874A Pending CN101486456A (en) | 2008-01-17 | 2008-01-17 | Industrial novel method for synthesizing fluorizated petroleum coke |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102420328A (en) * | 2010-09-28 | 2012-04-18 | 大金工业株式会社 | Positive electrode active material for lithium primary cell |
CN110875475A (en) * | 2018-09-04 | 2020-03-10 | 天津大学 | Method for preparing high-specific-energy carbon fluoride anode material by gas-phase fluoridation of fruit shell carbon |
-
2008
- 2008-01-17 CN CNA2008100327874A patent/CN101486456A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102420328A (en) * | 2010-09-28 | 2012-04-18 | 大金工业株式会社 | Positive electrode active material for lithium primary cell |
CN110875475A (en) * | 2018-09-04 | 2020-03-10 | 天津大学 | Method for preparing high-specific-energy carbon fluoride anode material by gas-phase fluoridation of fruit shell carbon |
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Addressee: Zhu Yaoping Document name: Notification of Publication of the Application for Invention |
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WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090722 |