Synthesis of fluorographite

Claim 2

A PROCESS OF PREPARING CARBON FLUORIDES COMPRISING THE STEPS OF: FIRST TREATING RELATIVELY SUBSTANTIALLY PURE CARBON WITH SUBSTANTIALLY ANHYDROUS HYDROGEN FLUORIDE AT A TEMPERATURE IN THE RANGE OF 200*-350*C. FOR A PERIOD OF 2 TO 3 HOURS, THEN FLUSHING THE SAID HYDROGEN FLUORIDE-TREATED CARBON WITH AN INERT GAS COMPRISING ONE OF THE CLASS OF NITROGEN, ARGON OR HELIUM IN THE TEMPERATURE RANGE OF 300*-450*C. UNTIL THE EXITING GASES ARE SUBSTANTIALLY FREE OF HF, AND THEREAFTER REACTING THE SUBSTANTIALLY HYDROGEN FLUORIDEFREE CARBON WITH FLUORINE AT A TEMPERATURE IN THE RANGE OF 300*-6000*C. FOR A TIME PERIOD OF 12 TO 16 HOURS.

Claim 3

A process as in claim 1 wherein the carbon is in the form of graphite.

Claim 4

A process as in claim 1 wherein the carbon is one of the non-crystalline forms.

Claim 5

A process as in claim 1 wherein the carbon is of 95% or higher percent purity, preferably over 95%.

Claim 6

A process as in claim 1 wherein the first anhydrous HF treatment is in the temperature range of 250*-310* C.

Claim 7

A process as in claim 1 wherein the carbon is first placed in a reactor preheated in the temperature range of approximately 300*-400* C,. anhydrous HF gas thereafter being passed over the carbon with the temperature of the reactor and its contents maintained in the range of 200*-350* C.

Claim 8

A process as in claim 1 including the additional step of a first, relatively short time fluorine treatment of the inert gas flushed hydrogen fluoride treated carbon wherein the said first fluorine treatment is continued for only 15 to 30 minutes with the reactor temperature rising to 300*-500* C, the reactor then being flushed with dry inert gas immediately after said first short term fluorine treatment, thereby somewhat lowering the reactor temperature, until same is free of smoke, anhydrous HF and fluorine.

Claim 9

A process as in claim 1 wherein the substantially hydrogen fluoride free carbon is treated with a combined fluorine and inert gas flow until an excess of fluorine over the theoretical amount is used.

Claim 10

A process as in claim 1 wherein a snow-white product essentially C1F1.26 is produced by reacting the substantially hydrogen fluoride free graphite with fluorine in the temperature range of 550* to 600* C.

Claim 11

A process as in claim 1 wherein a snow white product essentially C1F1.18 to C1F1.26 is produced by reacting the substantially hydrogen fluoride free non-crystalline carbon such as carbon black with fluorine in the temperature range of 300* to 400* C.

Claim 12

A process as in claim 1 wherein a vacuum is drawn on the reactor after treating the hydrogen fluoride treated graphite with an inert gas and before reacting same with fluorine.

Claim 13

A process as in claim 1 wherein the first 6 to 8 hours of fluorination are carried out at a reaction temperature between 510* to 550* C., the temperature thereafter lowered and maintained at 450* C. or below.

Claim 14

A process as in claim 1 wherein the first 6 to 8 hours of fluorination are carried out at a reaction temperature between 510* to 550* C., the temperature thereafter raised into the range of 550* to 600* C.

Claim 15

A process of preparing carbon fluorides comprising the steps of: placing a quantity of finely divided carbon in a liquid tight container; adding a molar excess of liquid anhydrous hydrogen fluoride to said carbon to said container; thoroughly mixing together the liquid anhydrous HF and finely divided carbon in the container and permitting the HF and carbon to soak together for at least substantially an hour; pouring off the excess HF from the HF damp carbon; heating the HF damp carbon in a reaction vessel at a temperature in the range of 200* to 350* C. for a period of 2 to 3 hours; then flushing the said HF-treated carbon with an inert gas comprising one of the class of nitrogen, argon or helium in the temperature range of 300*-450* C. until the exiting gases are substantially free of HF; and thereafter reacting the substantially hydrogen fluoride-free carbon with fluorine at a temperature in the range of 300*-600* C for a time period of 12 to 16 hours.

Claim 16

A process of preparing carbon fluorides comprising the steps of: placing a quantity of finely divided carbon in a liquid tight container; adding a molar excess of liquid anhydrous hydrogen fluoride to said carbon to said container; thoroughly mixing together the liquid anhydrous HF and finely divided carbon in the container and permitting the HF and carbon to soak together for at least substantially an hour; pouring off the excess HF from the HF damp carbon; heating the HF damp carbon in a reaction vessel at a temperature in the range of 200* to 350* C. for a period of 2 to 3 hours; then flushing the said HF-treated carbon with an inert gas comprising one of the class of nitrogen, argon or helium in the temperature range of 300*-450* C. until the exiting gases are substantially free of HF; and thereafter reacting the substantially hydrogen fluoride-free carbon with fluorine at a temperature in the range of 300*-600* C for a time period of 12 to 16 hours.

Claim 17

A process of preparing carbon fluoride of the composition C1F1.26 from graphite comprising the steps of first treating substantially pure graphite with substantially anhydrous hydrogen fluoride at a temperature in the range of 260*-310* C for a period of 2 to 3 hours; then flushing the said hydrogen fluoride-treated graphite with an inert gas in the temperature range of 310*-450* C until same is free of HF; thereafter reacting the substantially hydrogen fluoride-free graphite with fluorine at a temperature in the range of 450* t0 500* C for approximately 15 minutes; thereafter flushing the fluorine-treated graphite with an inert gas until the same is free from HF; and thereafter reacting the graphite with fluorine at a temperature in the range of 550*-600* C for a time period of 12 to 16 hours in order to obtain C1F1.26.

Claim 18

A process of preparing carbon fluoride of the composition C1F1.26 from graphite comprising the steps of first treating substantially pure graphite with substantially anhydrous hydrogen fluoride at a temperature in the range of 260*-310* C for a period of 2 to 3 hours; then flushing the said hydrogen fluoride-treated graphite with an inert gas in the temperature range of 310*-450* C until same is free of HF; thereafter reacting the substantially hydrogen fluoride-free graphite with fluorine at a temperature in the range of 450* t0 500* C for approximately 15 minutes; thereafter flushing the fluorine-treated graphite with an inert gas until the same is free from HF; and thereafter reacting the graphite with fluorine at a temperature in the range of 550*-600* C for a time period of 12 to 16 hours in order to obtain C1F1.26.

Claim 19

A process as in claim 15 wherein the second fluorine treatment takes place in the range of 16 hours until the product is substantially snow-white.

Claim 20

A process of preparing carbon fluoride of the composition C1F1.26 from carbon black comprising the steps of: first treating substantially pure carbon black with substantially anhydrous hydrogen fluoride at a temperature in the range of 260*-310* C for a period of 2 to 3 hours; thereafter flushing the said HF-treated carbon black with an inert gas at approximately 300* C until same is free from HF; thereafter reacting the substantially HF free carbon black with fluorine at a temperature in the range of 290*-300* C for a time period of 12 to 16 hours; thereafter again treating the now fluorine-treated carbon black with hydrogen fluoride in the temperature range of 260*-310* C for a period of 2 to 3 hours; thereafter treating the twice HF-treated carbon black with an inert gas at a temperature of approximately 300* C until same is substantially free of HF; and thereafter reacting the substantially HF-free carbon black with fluorine at approximately 300* C for a time period of 12 to 16 hours to produce C1F1.26.

Claim 21

A process of preparing carbon fluoride of the composition C1F1.26 from carbon black comprising the steps of: first treating substantially pure carbon black with substantially anhydrous hydrogen fluoride at a temperature in the range of 260*-310* C for a period of 2 to 3 hours; thereafter flushing the said HF-treated carbon black with an inert gas at approximately 300* C until same is free from HF; thereafter reacting the substantially HF free carbon black with fluorine at a temperature in the range of 290*-300* C for a time period of 12 to 16 hours; thereafter again treating the now fluorine-treated carbon black with hydrogen fluoride in the temperature range of 260*-310* C for a period of 2 to 3 hours; thereafter treating the twice HF-treated carbon black with an inert gas at a temperature of approximately 300* C until same is substantially free of HF; and thereafter reacting the substantially HF-free carbon black with fluorine at approximately 300* C for a time period of 12 to 16 hours to produce C1F1.26.

Claim 22

A process as in claim 17 wherein the second fluorine treatment is carried out for approximately 14 to 16 hours until the product is substantially snow-white.

Claim 23

Carbon fluoride of the composition C1F1.26 prepared from graphite comprising a snow white powder which, in an atmosphere of nitrogen is stable up to 650* C, showing slight decomposition at 662* C and complete decomposition at 737* C, same of turbostratic structure and having an inter-layer spacing of 6.03A.

Claim 24

Carbon fluoride of the composition C1F1.26 prepared from graphite comprising a snow white powder which, in an atmosphere of nitrogen is stable up to 650* C, showing slight decomposition at 662* C and complete decomposition at 737* C, same of turbostratic structure and having an inter-layer spacing of 6.03A.

Claim 25

The carbon fluoride of structure C1F1.26 prepared from carbon black which is a snow white powder having a stability in an atmosphere of nitrogen of around 400* C with decomposition starting around 340* C, same of amorphous structure and having an inter-layer spacing of 6.7A.

Claim 26

The carbon fluoride of structure C1F1.26 prepared from carbon black which is a snow white powder having a stability in an atmosphere of nitrogen of around 400* C with decomposition starting around 340* C, same of amorphous structure and having an inter-layer spacing of 6.7A.

Claim 27

Carbon fluoride as in claim 19 which is prepared by the steps of: first treating substantially pure graphite with substantially pure anhydrous hydrogen fluoride at a temperature in the range of 260*-310* C. for a period of 2 to 3 hours; then flushing the said hydrogen fluoride-treated graphite with an inert gas in the temperature range of 310*-450C. until same is free from HF; thereafter reacting the substantially hydrogen fluoride free graphite with fluorine at a temperature in the range of 450*-500* C. for approximately 15 minutes; thereafter flushing the fluorine-treated graphite with an inert gas until same is free from HF; and thereafter reacting the graphite fluorine at a temperature in the range of 550*-600* C. for a time period of 12 to 16 hours in order to obtain C1F1.26.

Claim 28

Carbon fluoride as in claim 20 prepared by a process comprising the steps of: first treating substantially pure carbon black with substantially anhydrous hydrogen fluoride at a temperature in the range of 260*-310* C. for a period of 2 to 3 hours; thereafter flushing the said HF-treated carbon black with an inert gas at approximately 300* C. until same is free from HF; thereafter reacting the substantially HF free carbon black with fluorine at a temperature in the range of 290*-300* C. for a time period of 12 to 16 hours; thereafter again treating the now fluorine-treated carbon black with hydrogen fluoride in the temperature range of 260*-310* C. for a period of 2 to 3 hours; thereafter treating the twice HF-treated carbon black with an inert gas at a temperature of approximately 300* C until same is substantially free of HF; and reacting the substantially HF-free carbon black with fluorine at approximately 300* C. for a time period of 12 to 16 hours to produce C1F1.26.