CN88105518A - Method of synthesis of poly-fluorocarbons - Google Patents
Method of synthesis of poly-fluorocarbons Download PDFInfo
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- CN88105518A CN88105518A CN 88105518 CN88105518A CN88105518A CN 88105518 A CN88105518 A CN 88105518A CN 88105518 CN88105518 CN 88105518 CN 88105518 A CN88105518 A CN 88105518A CN 88105518 A CN88105518 A CN 88105518A
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Abstract
Method of synthesis of poly-fluorocarbons of the present invention, be under 20-150 ℃ of temperature, to react by the gas mixture of fluorine gas and rare gas element and unformed coke with high-activity function, the productive rate of product poly-fluorocarbons can reach more than 96%, reacts safe and reliable, the danger of no combustion explosion.
Description
The present invention is the synthetic method that belongs to the organic fluorine carbon compound.
After this century, late nineteen seventies was found the application of poly-fluorocarbons in manufacturing fluorine/lithium high-energy battery, this compound had caused people's extensive interest.With poly-fluorocarbons is that the fluorine/lithium cell of raw material has good low-temperature performance, stable discharge performance and be equivalent to common batteries 8-10 energy density doubly, and storage period is long.In addition, poly-fluorocarbons can also be as application such as lubricants.
The synthetic method report of poly-fluorocarbons is a lot, according to [J.Chem.Soc.Dalton Trans.12,1268(1974)] fluorine and graphite reaction generation poly-fluorocarbons under the high temperature of more than 600 degree Celsius such as R.J.Lagow.According to Japanese Patent (J7518395,1975) report, the burnt reaction under 350 ℃ of temperature synthesized poly-fluorocarbons after employing was diluted fluorine gas and forged again.In above-mentioned known synthetic method, the carbon raw material is to adopt graphite or forge back Jiao, and reaction all is to carry out under comparatively high temps, reacts dangerous, the normal danger that combustion explosion easily takes place, and productive rate is also lower.
In order to overcome the shortcoming of above-mentioned known synthetic method, the present invention seeks to seek a productive rate height, the reaction conditions gentleness is controlled easily, and the method for synthesis of poly-fluorocarbons of combustion explosion phenomenon does not take place.
The synthetic method of poly-fluorocarbons of the present invention, the material mixed gas of forming by fluorine gas and rare gas element, flow through and place the amorphous coke that has high-activity function in the reactor, come in contact reaction with it, temperature of reaction is 20-150 ℃, product poly-fluorocarbons productive rate can reach more than 96%, and phenomenons such as combustion explosion do not take place during reaction.
The inventive method is fluorine gas and rare gas element with 1: 1 to 1: 8 mol ratio, and the optimal molar ratio example is 1: 1 to 1: 5, enters mixing tank constitutive material gas mixture, is metered into reactor through under meter.Temperature of reaction is 20-150 ℃, and optimal reaction temperature is 40-110 ℃, and reactor is a reaction tubes, because temperature of reaction is lower, so the material of reaction tubes can be metal or alloy (for example nickel, copper, iron, stainless steel etc.), silica glass etc.Also can be placed with a bateau made from same material in the pipe, the even amorphous coke powder of shakedown skim in the boat.Pipe external application electric furnace carries out temperature regulation.One temperature survey pipe is housed in the reaction tubes, and pipe end should be as far as possible near the coke bisque, so that can correctly measure temperature of reaction in reaction.
The rare gas element that is used to dilute fluorine gas can be nitrogen, carbonic acid gas, argon gas, helium, (carbon is from C for perfluoro-carbon
1-C
8) etc.
Amorphous coke powder is the decolorizing carbon with high-activity function, as refinery coke, coal tar, pitch coke, carbon black etc.Its true specific gravity is that 0.6-1.8 and granularity are the 60-400 order.
The mol ratio of raw material fluorine and coke is 〉=1, and for fear of the waste of fluorine gas, the optimal molar ratio example is 1-1.7.The gas mixture air-flow of fluorine gas and rare gas element comes in contact reaction with the flow of the 90-250 ml/min reaction tubes of flowing through with amorphous coke powder, and the reaction times is 2-15 hour.After the tail gas of reaction is removed toxic substance by alkaline absorbent (sodium hydroxide or potassium hydroxide solution) is emptying.The fluorine carbon ratio of reaction product poly-fluorocarbons is 0.8-1.25.When the fluorine carbon ratio is 0.8 to less than 1 the time, product is a white-yellowish solid, when the fluorine carbon ratio is 1-1.25, product is a white solid, but can both be used to make fluorine/lithium high-energy battery equally, the energy density that its difference is the former is low slightly than the latter's, thus fluorine carbon ratio the best of product be 〉=1.
The advantage of method of synthesis of poly-fluorocarbons of the present invention is that temperature of reaction is lower, and mild condition is easy to control, the danger of no combustion explosion, and safe and reliable, equipment is simple, and cost is lower, and productive rate can be up to more than 96%.
In order to understand the present invention better, now be exemplified below:
Example 1
Taking by weighing 12 gram granularities is the 80-150 order, and proportion is that 1.6 amorphous coke powder is layered in the bateau, in the reactor of packing into, reactor is vacuumized, and vacuum valve is shut in 130 ℃ of furnace temperature controls.28.5 the gram fluorine is that 1: 5 mixed becomes material mixed gas with fluorine and nitrogen mole ratio, flow with 150 ml/min feeds reactor, comes in contact reaction with unformed coke powder, reacts to get product white solid poly-fluorocarbons 32 grams after 11.2 hours, its fluorine carbon ratio is 1.05, and productive rate is 100%.
Example 2
Taking by weighing 12 gram granularities is the 200-250 order, and proportion is that 1.2 amorphous coke powder is layered in the bateau, in the reactor of packing into, reactor is vacuumized, and vacuum valve is shut in 60 ℃ of furnace temperature controls.21 gram fluorine are that 1: 2 mixed becomes material mixed gas with fluorine and helium mole ratio, and the flow feeding reactor with 120 ml/min comes in contact reaction with amorphous coke powder, react after 5.2 hours, get product white solid poly-fluorocarbons 31 grams, its fluorine carbon ratio is 1.0, and productive rate is 100%.
Example 3
Taking by weighing 24 gram granularities is the 150-200 order, and proportion is that 1.5 amorphous coke powder is layered in the bateau, in the reactor of packing into, reactor is vacuumized, and vacuum valve is shut in 100 ℃ of furnace temperature controls.45.6 the gram fluorine is that 1: 1 mixed becomes material mixed gas with fluorine and nitrogen mole ratio, flow with 90 ml/min feeds reactor, come in contact reaction with amorphous coke powder, react after 10 hours, get product white solid poly-fluorocarbons 62.8 grams, its fluorine carbon ratio is 1.08, and productive rate is 96.6%.
Example 4
Taking by weighing 12 gram granularities is the 350-400 order, and proportion is that 0.8 amorphous coke powder is layered in the bateau, in the reactor of packing into, reactor is vacuumized, and vacuum valve is shut in 30 ℃ of furnace temperature controls.21 gram fluorine are that 1: 2 mixed becomes material mixed gas with fluorine and tetrafluoro-methane mole ratio, flow with 180 ml/min feeds reactor, come in contact reaction with amorphous coke powder, react after 3.4 hours, get product white-yellowish solid carbon monofluoride 30.2 grams, its fluorine carbon ratio is 0.96, and productive rate is 100%.
Claims (8)
1, a kind of material mixed gas and carbon of being made up of fluorine gas and rare gas element reacts the method for synthesizing poly-fluorocarbons, it is characterized in that temperature of reaction is 20-150 ℃, the carbon raw material is the amorphous coke with high-activity function, the mol ratio of raw material fluorine and carbon is 〉=1, and the mol ratio of fluorine gas and rare gas element is 1.1-1.8.
2, the synthetic method of newly stating by claim (1) is characterized in that optimal reaction temperature is 40-110 ℃.
3, by the described synthetic method of claim (1), the amorphous coke that it is characterized in that having high-activity function is a refinery coke, coal tar, pitch coke, carbon black etc.
4, by the described synthetic method of claim (3), the true specific gravity that it is characterized in that amorphous coke is 0.6-1.8.
5, by the described synthetic method of claim (3), the granularity that it is characterized in that amorphous coke is the 60-400 order.
6, by the described synthetic method of claim (1), it is characterized in that rare gas element is a nitrogen, carbonic acid gas, argon gas, helium, (carbon is from C for perfluoro-carbon
1-C
8) etc.
7,, it is characterized in that the optimal molar ratio example of raw material fluorine and carbon is 1-1.7 by the described synthetic method of claim (1).
8,, it is characterized in that the optimal molar ratio example of fluorine gas and rare gas element is 1.1-1.5 by the described synthetic method of claim (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105518 CN88105518A (en) | 1988-05-10 | 1988-05-10 | Method of synthesis of poly-fluorocarbons |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105518 CN88105518A (en) | 1988-05-10 | 1988-05-10 | Method of synthesis of poly-fluorocarbons |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN88105518A true CN88105518A (en) | 1988-12-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88105518 Pending CN88105518A (en) | 1988-05-10 | 1988-05-10 | Method of synthesis of poly-fluorocarbons |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108927191A (en) * | 2017-05-22 | 2018-12-04 | 天津大学 | Fluorine-containing graphite-phase nitrogen carbide photochemical catalyst and preparation method thereof |
-
1988
- 1988-05-10 CN CN 88105518 patent/CN88105518A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108927191A (en) * | 2017-05-22 | 2018-12-04 | 天津大学 | Fluorine-containing graphite-phase nitrogen carbide photochemical catalyst and preparation method thereof |
| CN108927191B (en) * | 2017-05-22 | 2021-05-28 | 天津大学 | Fluorine-containing graphite phase nitrogen carbide photocatalyst and preparation method thereof |
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