Method of producing graphite fluoride

专利摘要:
A graphite fluoride comprising mainly poly-dicarbon monofluoride represented by the formula (C2F)n can be produced in an extremely short period of time by a process comprising reacting a graphite material with fluorine in the presence of a specific fluoride.
公开号:SU1190982A3
申请号:SU823381403
申请日:1982-01-27
公开日:1985-11-07
发明作者:Ватанабе Нобуацу；Накадзима Цуеси；Кавагути Масаюки
申请人:Эпплайд Сайенс Рисерч Институт И Нобуацу Ватанабе (Фирма)；
IPC主号:

专利说明:

The invention relates to methods for producing graphite fluoride, recommended for use as an active material in electrical cells, lubricants, water resistant staining to water and / or oil repellent, etc. The method of obtaining graphite fluoride is known (Formulas C P by processing graphite using a pro- 500 c Ij However, this method is very sophisticated. The purpose of the invention is to reduce the duration of the process. The goal is achieved by the fact that according to the method of processing graphite powder fluorine at 300-500 ° C, the treatment is carried out in the presence of fluoride of an element selected from the group consisting of lithium, magnesium, calcium, aluminum, chromium, manganese, cobalt, iron, copper and zinc. Graphite and fluoride of the selected element contacted with fluorine at a temperature of from room temperature to 100 ° C and then heated to 300-500 ° C. Contact with fluorine is carried out for min-20h, anheating is up to 300-500 ° C with a speed of 2-100 degrees / mic Typically fluorite is graphite to achieve a constant weight of the product. In the presence of lithium, magnesium, kalidium, aluminum, chromium, manganese, cobalt, iron, copper, or zinc fluorides, the reaction is significantly accelerated. Contacting graphite and fluoride of an element with fluorine and subsequent heating under these conditions will further intensify the process. In this case, the deviation from these modes leads to a slowing down of the fluorination process. The separation of graphite fluoride produced from the use of fluoride elements is carried out, for example, in water, by the method according to the flotation method, since (Cj, F) has water-repellent properties. When using fluoride gas, separation is easier. Example 1. A mixture of 50 mg of Madagascar flake natural graphite with a particle size of 16 (0.991 mm) or more and 50 mg of AlFg is placed into a monel reactor. Fluorine is introduced into the reactor at room temperature and a pressure of 760 mm Hg. (the time of introduction of fluorine is 5 minutes), the reaction system is heated to 400 ° C at a temperature rise rate of 30 K / min. At this temperature, the reaction continues for 5 hours. Graphite fluoride is obtained, which is gray in color and has an F / C ratio of 0.677, with a yield of 100% relative to the used graphite. Example 2. Preparation of graphite fluoride is carried out analogously to example 1, except that after the introduction of fluorine, the reaction system is heated to 100 ° C, held for 0.5 h, and then heated to 400 ° C at a rate of 2.5 degrees / min At 400 ° C, the reaction is continued for 9 hours. Gray graphite fluoride is obtained with an F / C ratio of 0.601 and a yield of 100% relative to the graphite used. Sample S-13 and 18-25 and comparative example 4. The preparation of graphite fluoride is carried out analogously to example 2. The particle size of graphite, the type of fluoride element introduced, the contact and reaction times and the heating rate are changed to 300-500 0. The process data are shown in the table. Comparative example 1. The process is carried out analogously to example 1 except that. That AIF is not used. After VOh after the start of the reaction at 400 ° С, the product is examined by x-ray diffraction. In the powder X-ray diffraction pattern, a peak is still observed, due to the remaining unreacted carbon. Two weeks after the start of the reaction, graphite fluoride was obtained with an F / C ratio of 0.62, Examples 14-17 and Comparative Examples 2 and 3. The preparation of fluoride and graphite was carried out analogously to Example 2, except that heat-treated petroleum coke (Franklin number, 31, heat treatment at 2 for 30 minutes) with a particle size of 46 μm is used instead of natural graphite and the process conditions are changed. Graphite fluoride is obtained having an F / C ratio according to the table. The use of the invention makes it possible to shorten the process for producing graphite fluoride of the formula () by two or more times as compared with the known method.
year
N A
Sch1
p g
about with

what g
m
about
sh
about "g
oh oh
sf o
 I
l “a
cm
ech
A ro
VO
Yu
in
sh
about
1L
1L sc
cm
about oh sjsh
about
oh oh
.
Very good
1L
Yu
1P
"H
1L
cg
1L
to
with
about
ate
1L
in
in
.LO
about
oo
about
go g
00
00
sh
“Ъ go
P
1G |
about
about
about
ABOUT
SP
00
Yu
si1L
g
Yu
"%
""
1F 4f
ABOUT
g
About VO
00
Cho
VO. l
ABOUT
1L
um
D) ate
about
th 00 th
about
about
00 th
1O
1L
go
Yu
"T
about
1L
1L
in
l
VO
one
"K with
go
Cvj
in
in
iN
in
"
-
VO
VO

"Ъ
about
GO
with
with
1G)
about
about: about
tf in
mo
N o
fe o
fego (x (.with
m "
 SG
about
w oh
in about
(M
cm
BUT
cm
"
about
about
about
go
go
go go
vO
"K
go go
about
-
1L
Ltd
oo
about
about
 l
oh oh
CN
go
Cho
vO
vO
vO
R in

in about
- about
about
- about
about
chg about
about
about
go
about go
go
ъ And
about
oh oh
about
oh oh
go ksI
, lr.
I w
Sd
Software) 2
 but
P)
.а Sa ft
vO
and S2 p,
oh and in tM
about sb and
about
vO
About VO
I
with
00
YU
CJ
ABOUT
about es
vO
"I
with
vD
1L
/
00
R.;
V
 about
ABOUT
o ech
ABOUT
about with
"L
and oh oh
with
"P
s
0)
cc

权利要求:
Claims (3)
[1]
1. THE METHOD FOR PRODUCING GRAPHITE FLUORIDE of the formula (C ₂ F) _n , including the treatment of graphite powder with fluorine at 300-500 ° C, is distinguished by the fact that, in order to reduce the duration of the process, the treatment is carried out in the presence of fluoride of the element selected from the group consisting of lithium, magnesium, calcium, aluminum, chromium, manganese, cobalt, iron, copper and zinc.
[2]
2. The method of claim 1, wherein the graphite and fluoride of the selected element are contacted with fluorine at a temperature of from room temperature to 100 ° C and then heated to 300500 ° C.
[3]
3. The method according to p. 2, characterized in that the contacting with fluorine is carried out for 1 minute - 20 hours, and heating to 300-500 C at a speed of 2-100 deg / min.
>

类似技术:

---

公开号 | 公开日 | 专利标题

---

SU1190982A3|1985-11-07|Method of producing graphite fluoride

---

US6022404A|2000-02-08|Surface-modified, pyrogenically produced mixed oxides, method of their production and use

---

RU2049099C1|1995-11-27|Method of producing rutile titanium dioxide pigment

---

EP0134643A2|1985-03-20|Preparing metallic zirconium, hafnium or titanium

---

DE3227041A1|1983-02-10|METHOD FOR PRODUCING A GRAPHITE FLUORIDE

---

JP2974540B2|1999-11-10|Purification method of fluoroalkylsulfonic acid

---

JP3437970B2|2003-08-18|Method for producing hydroxyapatite

---

JPH03193793A|1991-08-23|Production of tris|phosphate

---

WO1989010327A2|1989-11-02|Synthesis of carbon fluoride and carbon fluoride chloride

---

JPH061614A|1994-01-11|Compound expressed by formula bi5o7no3 and its production

---

JP2828349B2|1998-11-25|Method for producing tin trifluoromethanesulfonate

---

EP0464369A1|1992-01-08|Process for the preparation of aluminium nitride

---

SU990664A1|1983-01-23|Process for producing magnesium fluoride

---

SU1590433A1|1990-09-07|Method of producing manganese, cobalt, nickel or zinc difluoride

---

SU880980A1|1981-11-15|Method of producing sodium fluoride

---

SU975577A1|1982-11-23|Process for producing titanium dioxide pigment of the anatase modification

---

JPH0234512A|1990-02-05|Zeolite of novel mtt structural type and its synthesis method

---

SU1490869A1|1991-04-23|Method of producing diamond powders

---

SU715555A1|1980-02-15|Method of preparing superphosphate

---

SU1505958A1|1989-09-07|Clayless drilling mud and method of producing same

---

EP0251155B1|1991-03-27|A method of manufacturing barium sulphide

---

Jemal et al.2004|Preparation, characterization and thermal behaviour of samarium | cyclotriphosphate |, SmP3O9· 5H2O

---

McCullough et al.1954|A new synthesis of 1, 4-diselenane. The 1, 1, 4, 4-diselenane tetrahalides

---

Cevasco et al.1991|The E1cB mechanism in the alkaline hydrolysis of N, N-diethyl-P-| phosphonamidic chloride

---

Christe et al.1987|Preparation and characterization of Ni | 2

同族专利:

---

公开号 | 公开日

---

JPS6220127B2|1987-05-06|

---

IT1150602B|1986-12-17|

---

FR2512429A1|1983-03-11|

---

IT8219278D0|1982-01-25|

---

GB2106882A|1983-04-20|

---

FR2512429B1|1985-10-25|

---

US4423261A|1983-12-27|

---

NL8200160A|1983-04-05|

---

JPS5845104A|1983-03-16|

---

DE3201116A1|1983-03-17|

---

GB2106882B|1985-02-06|

---

DE3201116C2|1987-02-05|

引用文献:

---

公开号 | 申请日 | 公开日 | 申请人 | 专利标题

---

---

US2770660A|1952-02-11|1956-11-13|Kellogg M W Co|Method of producing fluorocarbons|

---

JPS595523B2|1972-02-14|1984-02-06|Nippon Carbon Co Ltd|

---

US3929918A|1972-10-06|1975-12-30|Ozark Mahoning Co|Synthesis of fluorographite|

---

JPS542918B2|1973-05-30|1979-02-15|

---

US3929920A|1973-05-31|1975-12-30|Daikin Ind Ltd|Process for continuous fluorination of carbon|

---

GB1460240A|1974-11-12|1976-12-31|Exxon Research Engineering Co|Lewis acid-fluorine compounds of carbon|

---

US4083885A|1975-09-02|1978-04-11|Mobil Oil Corporation|Alkylation with catalyst of graphite containing intercalated fluoride|

---

JPS612609B2|1977-02-22|1986-01-27|Oyo Kagaku Kenkyusho|

---

US4243615A|1977-02-22|1981-01-06|Watanabe Applied Science Research Institute|Process for preparing poly-dicarbon monofluoride|

---

JPS6142378B2|1978-08-21|1986-09-20|Oyo Kagaku Kenkyusho|JPS6110404B2|1981-07-22|1986-03-29|Central Glass Co Ltd|

---

US4477374A|1981-10-03|1984-10-16|Central Glass Co., Ltd.|Ternary intercalation compound of a graphite with a metal fluoride and fluorine, a process for producing the same, and an electrically conductive material comprising the ternary intercalation compound|

---

JPH0139965B2|1982-09-10|1989-08-24|Central Glass Co Ltd|

---

JPH0413289B2|1983-03-09|1992-03-09|Watanabe N|

---

JPS6068559A|1983-09-24|1985-04-19|Central Glass Co Ltd|Active material for battery|

---

US4556618A|1983-12-01|1985-12-03|Allied Corporation|Battery electrode and method of making|

---

JPH0677458B2|1984-11-12|1994-09-28|信淳 渡辺|Battery active material|

---

FR2609286B1|1987-01-05|1989-03-17|Atochem|CONTINUOUS PROCESS FOR THE PREPARATION OF CARBON POLYMONOFLUORIDE AND APPARATUS FOR IMPLEMENTING SAME|

---

US4886921A|1988-04-18|1989-12-12|Allied-Signal Inc.|Synthesis of carbon fluoride and carbon fluoride chloride|

---

US4795624A|1988-04-28|1989-01-03|Allied-Signal Inc.|Low temperature synthesis of graphite based carbon fluoride and carbon fluoride chloride|

---

JPH0222114A|1988-07-11|1990-01-25|Daikin Ind Ltd|Purification of fluorocarbon|

---

US4957661A|1988-09-30|1990-09-18|The United States Of America As Represented By The United States National Aeronautics And Space Administration|Graphite fluoride fiber polymer composite material|

---

US5286471A|1992-05-15|1994-02-15|The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration|Graphite flouride from iodine intercalated graphitized carbon|

---

US5622683A|1994-06-13|1997-04-22|Hung; Ching-Cheh|Chemically modified carbonaceous materials made by the defluorination of graphite fluoride and process therefor|

---

FR2748014B1|1996-04-26|1998-07-17|Centre Nat Rech Scient|NOVEL FLUORINATED CARBONES, THEIR PREPARATION PROCESS AND THEIR USE AS ELECTRODE MATERIAL|

---

US9029019B2|2007-08-17|2015-05-12|Nanotek Instruments, Inc.|Carbon anode compositions for lithium ion batteries|

---

US7993780B2|2007-10-05|2011-08-09|Nanotek Instruments, Inc.|Process for producing carbon anode compositions for lithium ion batteries|

---

BR112012002587A2|2009-08-07|2016-03-22|Blacklight Power Inc|power source, power system, fuel cell system or battery.|

---

CN105621398B|2015-12-25|2019-08-27|山东重山光电材料股份有限公司|A kind of method that catalysis method prepares high-purity fluorographite|

---

CN108439367B|2018-06-22|2021-09-07|湖北卓熙氟化股份有限公司|Method for preparing nano graphite fluoride at low temperature|

---

CN108622892B|2018-06-22|2021-09-07|湖北卓熙氟化股份有限公司|Method for preparing graphite fluoride at low temperature|

---

CN109319772A|2018-10-23|2019-02-12|湖北工程学院|A kind of porous fluorinated graphene and preparation method thereof, application|

法律状态:

优先权:

---

申请号 | 申请日 | 专利标题

---

JP56143007A|JPS6220127B2|1981-09-10|1981-09-10|

---