CN1887832A - Large scale synthesis process of carbon fluorides - Google Patents
Large scale synthesis process of carbon fluorides Download PDFInfo
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- CN1887832A CN1887832A CN 200510027218 CN200510027218A CN1887832A CN 1887832 A CN1887832 A CN 1887832A CN 200510027218 CN200510027218 CN 200510027218 CN 200510027218 A CN200510027218 A CN 200510027218A CN 1887832 A CN1887832 A CN 1887832A
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Abstract
The present invention is large scale synthesis process of carbon fluoride as one new type of functional material. Carbon fluoride material is white or grey, non-toxic, nonflammable, non-corrosive and chemically stable. It may be used as insulating material, waterproofing material, lubricant material and electrode material for high energy lithium battery, and has excellent performance and superiority of being used in the conditions of high temperature, high pressure, high load, strong acid and alkali environment. Carbon fluoride material is prepared through introducing fluorine gas or mixed gas of fluorine and nitrogen or other inert gas into special solidifying bed with various kinds of carbon process so as to produce reaction in certain temperature to generate carbon fluoride product of different sizes.
Description
Technical Field
The series of carbon fluoride products are novel functional materials and have wide application; the material is white or gray in a normal state, is non-toxic, non-flammable, non-corrosive and stable in chemical property, and is a good insulating material, a goodwaterproof material and a good lubricating material; the lithium ion battery can be used as an electrode material of a novel high-energy lithium battery, the battery is very prominent in the aspects of high energy, safety and stability, long service life, energy conservation, environmental protection and the like, and is a new generation of safe, energy-saving and environment-friendly high-energy battery; the lubricant has better lubricity than solid lubricants such as graphite, molybdenum disulfide and the like, has more outstanding superiority particularly under severe conditions such as high temperature, high pressure, high load, strong acid, strong alkali environment and the like, can be widely applied to high-speed airplanes, carrier rockets, missiles, tanks, automobiles and the like as the lubricant, and is called as an epoch-making novel solid lubricant by foreign experts.
Background
At present, the product attracts great attention and is widely applied in developed countries such as the Nissan America and the Russia, and the excellent high-temperature lubricating property enables the product to become a pet for national defense and military industry of various countries; the well-known panasonic corporation of japan has developed a new type of high-energy lithium battery using carbon fluoride as a positive electrode, and the characteristics of safety, environmental protection and high energy are the best among all lithium batteries. The product can be produced in large scale in developed countries such as Nissan America and Russia; in China, the interest of the method is increasing day by day, but the technology for industrially producing the series of the carbon fluoride is not mature, and the method has a larger gap compared with the overseas peers. After long-time research on the products and dynamic tracking of related documents and self-designed reactors to carry out various test works, years of efforts make a breakthrough and a mature method for producing carbon fluoride on a large scale is developed.
Disclosure of Invention
The applicant herein claims a synthetic method for the mass production of a series of fluorocarbons, and the novel functional materials protected by this patent, a series of fluorocarbons and their specific synthetic procedures, are described as follows:
the compound synthesized by the invention is a series of carbon fluoride products, and the composition of the carbon fluoride products can be expressed by the following general formula:
CFxwherein x is more than 0 and less than 1.2;
raw materials of the reaction are petroleum coke, graphite, active carbon, carbon black or carbon fiber and other carbon-containing simple substances; the other raw material is fluorine gas or fluorine gas diluted by inert gas, the fluorine gas and the fluorine gas react in a special reaction container-a solidification bed of copper, nickel or monel material at a certain temperature to obtain a product, and the reaction formula is as follows:
the preparation of the series of fluorocarbons described in this patent was carried out as follows: firstly, adding a carbon-containing simple substance, and vacuumizing; secondly, heating the system to a specific reaction temperature. Thirdly, fluorine gas is introduced, and the fluorine gas and the carbon simple substance generate a plurality of kinds of carbon fluoride in the reaction container; fourthly, absorbing fluorine gas from the tail gas generated in the reaction process through two absorption cells filled with alkali liquor; and fifthly, opening the reaction kettle, taking out the carbon fluoride product in the reaction kettle, classifying the carbon fluoride product into different grades according to different colors, and carrying out appropriate post-treatment, namely separation treatment by a micro powder separation technology.
Detailed Description
The following examples illustrate the preparation of such fluorinated carbons as described in the present invention.
Example one:
adding 2-4Kg of petroleum coke into a fluidized bed, heating to about 200 ℃ under the condition that an oil pump vacuumizes for half an hour, filling nitrogen to expel air, and repeating for three times. Raising the temperature of the reaction kettle to 600 ℃, slowly introducing fluorine gas, controlling the flow rate of the fluorine gas added to be 300 ml/s through a fluorine gas flowmeter, continuing to react for 6-10 hours, stopping heating, naturally cooling the temperature of the reaction kettle to room temperature, introducing nitrogen gas into the reaction kettle cooled to room temperature, removing the residual fluorine gas in the reaction kettle, and finishing the reaction. In the reaction process, the gas outlet after passing through the reactor is connected to two absorption towers filled with potassium hydroxide or other alkali liquor to absorb the complete fluorine gas. Opening the reaction kettle, and taking out solid powder in the solidification bed, wherein most of the solid powder is offwhite powder and a small amount of black powder is also available; the product is treated by micro powder separation technology to obtain 3-6Kg of offwhite product with fluorine content of 61-64%.
Example two:
adding 2-4Kg of petroleum coke into a fluidized bed,heating to about 200 ℃ under the condition that an oil pump vacuumizes for half an hour, filling nitrogen to expel air, and repeating for three times. Raising the temperature of the reaction kettle to 500 ℃ below zero, slowly introducing fluorine gas, controlling the flow of the fluorine gas added to be 300 ml/s through a fluorine gas flowmeter, continuing to react for 4-8 hours, stopping heating, naturally cooling the temperature of the reaction kettle to room temperature, introducing nitrogen gas into the reaction kettle after the temperature of the reaction kettle is cooled to room temperature, removing the residual fluorine gas in the reaction kettle, and finishing the reaction. In the reaction process, the gas outlet after passing through the reactor is connected to two absorption towers filled with potassium hydroxide or other alkali liquor to absorb the complete fluorine gas. Opening the reaction kettle, and taking out solid powder in the solidification bed, wherein most of the solid powder is black powder and a small amount of off-white powder is also available; the product is treated by micro powder separation technology to obtain 0.5-1.0Kg of offwhite product with fluorine content of about 60%.
Example three:
adding 2-4Kg of graphite into the fluidized bed, heating to about 200 ℃ under the condition that an oil pump vacuumizes for half an hour, filling nitrogen to expel air, and repeating for three times. Raising the temperature of the reaction kettle to 500-600 ℃, slowly introducing mixed gas with the ratio of fluorine gas to nitrogen gas being 1: 1, controlling the flow of fluorine gas added to be 300 ml/s through a fluorine gas flowmeter, and continuously reacting for 6-10 hours; and stopping heating, naturally cooling the temperature of the reaction kettle to room temperature, introducing nitrogen into the reaction kettle which is cooled to the room temperature, driving away residual fluorine gas in the reaction kettle, andfinishing the reaction. In the reaction process, the gas outlet after passing through the reactor is connected to two absorption towers filled with potassium hydroxide or other alkali liquor to absorb the complete fluorine gas. Opening the reaction kettle, taking out the solid powder in the solid bed, obtaining 0.5-1.0Kg of gray product with fluorine content of about 55% through micro powder separation technology, wherein the color is darker and the reaction is not uniform.
Example four:
adding 2-4Kg of graphite into the fluidized bed, heating to about 200 ℃ under the condition that an oil pump vacuumizes for half an hour, filling nitrogen to expel air, and repeating for three times. Raising the temperature of the reaction kettle to 600-700 ℃, slowly introducing mixed gas with the ratio of fluorine gas to nitrogen gas being 1: 1, controlling the flow of fluorine gas added to be 300 ml/s through a fluorine gas flowmeter, continuing to react for 6-10 hours, stopping heating, naturally cooling the temperature of the reaction kettle to room temperature, introducing nitrogen gas into the reaction kettle cooled to room temperature, removing residual fluorine gas in the reaction kettle, and finishing the reaction. In the reaction process, the gas outlet after passing through the reactor is connected to two absorption towers filled with potassium hydroxide or other alkali liquor to absorb the complete fluorine gas. And opening the reaction kettle, taking out the solid powder in the fluidized bed, wherein the solid powder is light in color and relatively uniform in reaction, and treating the solid powder by a micro powder separation technology to obtain 3-5Kg of gray product with the fluorine content of about 58%.
Example five:
adding 2-4Kg of activated carbon into a curing bed, heating to about 200 ℃ under the condition that an oil pump vacuumizesfor half an hour, filling nitrogen to expel air, and repeating for three times. Raising the temperature of the reaction kettle to 400-600 ℃, slowly introducing fluorine gas, controlling the flow of the fluorine gas added to be 300 ml/s through a fluorine gas flowmeter, continuing to react for 6-10 hours, stopping heating, naturally cooling the temperature of the reaction kettle to room temperature, introducing nitrogen gas into the reaction kettle after the temperature of the reaction kettle is cooled to room temperature, removing the residual fluorine gas in the reaction kettle, and finishing the reaction. In the reaction process, the gas outlet after passing through the reactor is connected to two absorption towers filled with potassium hydroxide or other alkali liquor to absorb the complete fluorine gas. And opening the reaction kettle, taking out the solid powder in the fluidized bed, wherein the solid powder is light in color and relatively uniform in reaction, and treating the solid powder by a micro powder separation technology to obtain 3-5Kg of off-white product with the fluorine content of about 60%.
Example six:
adding 2-4Kg of carbon black into a fluidized bed, heating to about 200 ℃ under the condition that an oil pump vacuumizes for half an hour, filling nitrogen to expel air, and repeating for three times. Raising the temperature of the reaction kettle to 400-600 ℃, slowly introducing mixed gas with the ratio of fluorine gas to nitrogen gas being 1: 1, controlling the flow of fluorine gas added to be 300 ml/s through a fluorine gas flowmeter, continuing to react for 5-8 hours, stopping heating, naturally cooling the temperature of the reaction kettle to room temperature, introducing nitrogen gas into the reaction kettle cooled to the room temperature, removing residual fluorine gas in the reaction kettle, and finishing the reaction. In the reaction process, the gas outlet after passing through the reactor is connected to twoabsorption towers filled with potassium hydroxide or other alkali liquor to absorb the complete fluorine gas. And opening the reaction kettle, taking out the solid powder in the fluidized bed, wherein the solid powder is light in color and relatively uniform in reaction, and treating the solid powder by a micro powder separation technology to obtain 3-6Kg of gray product with the fluorine content of about 60%.
Example seven:
adding 2-4Kg of ink fiber into a curing bed, heating to about 200 ℃ under the condition that an oil pump vacuumizes for half an hour, filling nitrogen to expel air, and repeating for three times. Raising the temperature of the reaction kettle to 500-700 ℃, slowly introducing mixed gas with the ratio of fluorine gas to nitrogen gas being 1: 1, controlling the flow of fluorine gas added to be 300 ml/s through a fluorine gas flowmeter, continuing to react for 5-10 hours, stopping heating, naturally cooling the temperature of the reaction kettle to room temperature, introducing nitrogen gas into the reaction kettle cooled to room temperature, removing residual fluorine gas in the reaction kettle, and finishing the reaction. In the reaction process, the gas outlet after passing through the reactor is connected to two absorption towers filled with potassium hydroxide or other alkali liquor to absorb the complete fluorine gas. And opening the reaction kettle, taking out the solid powder in the fluidized bed, wherein the solid powder is light in color and relatively uniform in reaction, and treating the solid powder by a micro powder separation technology to obtain 3-6Kg of gray product with the fluorine content of about 63 percent.
Claims (11)
- A process for the large scale production of a series of fluorinated carbons is described. The carbon-containing raw material can be petroleum coke, graphite, activated carbon, carbon black or carbon fiber and the like; the other raw material can be fluorine gas, fluorine gas and nitrogen gas or mixed gas of fluorine gas and other inert gases; reacting the two in a special solidifying bed at 300.800 ℃, wherein the reacting bed is made of copper, nickel, Monel or the mixture thereof; each reaction can obtain 3.6 kg of carbon fluoride product, and the product can be CFxExpression (where 0<x<1.5). The product is white or gray in a normal state, is non-toxic, non-flammable, non-corrosive and stable in chemical property, and is a good insulating material, waterproof material and lubricating material; the lithium ion battery can be used as an electrode material of a novel high-energy lithium battery, the battery is very prominent in the aspects of high energy, safety and stability, long service life, energy conservation, environmental protection and the like, and is a new generation of safe, energy-saving and environment-friendly high-energy battery; the lubricating oil also has better lubricating property than solid lubricants such as graphite, molybdenum disulfide and the like, and particularly has more superior properties under severe conditions such as high temperature, high pressure, high load, strong acid, strong alkali environment and the like.
- 1. One raw material can be petroleum coke, graphite, activated carbon, carbon black or carbon fiber and the like; the other raw material can be fluorine gas, fluorine gas and nitrogen gas or mixed gas of fluorine gas and other inert gases;
- 2. reacting the two raw materials in a special solidifying bed at 300.800 ℃, wherein the reacting bed is made of copper, nickel, Monel or a mixed material thereof;
- 3. example one fluorinated carbon having the formula CFxWherein x is more than 0.9 and less than 1.2;
- 4. example two A fluorinated carbon of the formula CFxWherein x is more than 0 and less than 0.9;
- 5. example III A fluorinated carbon of the formula CFxWherein x is more than 0 and less than 0.8;
- 6. example four A fluorinated carbon of the formula CFxWherein x is more than 0.8 and less than 11;
- 7. example five A fluorinated carbon of the formula CFxWherein x is more than 0 and less than 1.2;
- 8. example six A fluorinated carbon of the formula CFxWherein x is more than 0 and less than 1.2;
- 9. example seven A fluorinated carbon having the formula CFxWherein x is more than 0 and less than 1.2;
- 10. 0-6 kg of carbon fluoride product can be obtained in each reaction, and the carbon fluoride product can be properly amplified for 10-100 kg/time and is used for large-scale production.
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| CN 200510027218 CN1887832A (en) | 2005-06-29 | 2005-06-29 | Large scale synthesis process of carbon fluorides |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730663A (en) * | 2012-06-13 | 2012-10-17 | 西北核技术研究所 | Carbon fluoride and application thereof |
| CN102903921A (en) * | 2012-10-31 | 2013-01-30 | 厦门大学 | Aqueous battery using carbon fluoride as anode |
| CN103332669A (en) * | 2013-06-14 | 2013-10-02 | 谢子卓 | Method for preparing carbon monofluoride or fluorocarbon through inner circulation of fluorine |
| CN104308142A (en) * | 2014-09-26 | 2015-01-28 | 湖北卓熙氟化股份有限公司 | Environment-friendly energy-saving mold release agent for powder metallurgy, and preparation method and application of environment-friendly energy-saving mold release agent |
| CN106941178A (en) * | 2017-05-12 | 2017-07-11 | 厦门希弗新能源科技有限公司 | A kind of fluorocarbons and its preparation method and application |
| CN107557125A (en) * | 2017-09-26 | 2018-01-09 | 中国石油化工股份有限公司 | A kind of PFPE type conductive grease and preparation method thereof |
| CN111003799A (en) * | 2019-12-31 | 2020-04-14 | 丽水学院 | Biological carrier for sewage treatment and preparation method thereof |
| CN112331848A (en) * | 2020-11-10 | 2021-02-05 | 厦门永力鑫新能源科技有限公司 | Carbon fluoride material with core-shell structure, preparation method thereof and lithium battery |
-
2005
- 2005-06-29 CN CN 200510027218 patent/CN1887832A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730663A (en) * | 2012-06-13 | 2012-10-17 | 西北核技术研究所 | Carbon fluoride and application thereof |
| CN102730663B (en) * | 2012-06-13 | 2014-11-26 | 西北核技术研究所 | Carbon fluoride and application thereof |
| CN102903921A (en) * | 2012-10-31 | 2013-01-30 | 厦门大学 | Aqueous battery using carbon fluoride as anode |
| CN102903921B (en) * | 2012-10-31 | 2015-09-02 | 厦门大学 | A kind of take fluorocarbons as the water system battery of positive pole |
| CN103332669A (en) * | 2013-06-14 | 2013-10-02 | 谢子卓 | Method for preparing carbon monofluoride or fluorocarbon through inner circulation of fluorine |
| CN104308142A (en) * | 2014-09-26 | 2015-01-28 | 湖北卓熙氟化股份有限公司 | Environment-friendly energy-saving mold release agent for powder metallurgy, and preparation method and application of environment-friendly energy-saving mold release agent |
| CN106941178A (en) * | 2017-05-12 | 2017-07-11 | 厦门希弗新能源科技有限公司 | A kind of fluorocarbons and its preparation method and application |
| CN107557125A (en) * | 2017-09-26 | 2018-01-09 | 中国石油化工股份有限公司 | A kind of PFPE type conductive grease and preparation method thereof |
| CN107557125B (en) * | 2017-09-26 | 2020-07-21 | 中国石油化工股份有限公司 | Perfluoropolyether conductive lubricating grease and preparation method thereof |
| CN111003799A (en) * | 2019-12-31 | 2020-04-14 | 丽水学院 | Biological carrier for sewage treatment and preparation method thereof |
| CN111003799B (en) * | 2019-12-31 | 2022-08-16 | 丽水学院 | Biological carrier for sewage treatment and preparation method thereof |
| CN112331848A (en) * | 2020-11-10 | 2021-02-05 | 厦门永力鑫新能源科技有限公司 | Carbon fluoride material with core-shell structure, preparation method thereof and lithium battery |
| CN112331848B (en) * | 2020-11-10 | 2021-10-26 | 厦门永力鑫新能源科技有限公司 | Carbon fluoride material with core-shell structure, preparation method thereof and lithium battery |
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