A method of obtaining a fluorinated carbon

 

(57) Abstract:

The invention is intended for the chemical industry and can be used to obtain lubricants, coatings, cathodic materials in chemical current sources. Charged to the reactor, a carbon material such as carbon black or thermobarometry graphite. The fluorination is carried out at 320 - 500oC with a mixture of nitrogen and technical fluorine from the fluorine content of 12%. The fluorination process is interrupted when the ratio of the concentration of fluorine in the gas at the exit and entrance of 0.5 - 0.6 by stopping the supply of the inert gas. The decomposition of the fluorocarbon fix the temperature rise in the reactor. Stop filing fluorine. After cooling the reactor to the temperature of the beginning of fluoridation resume the supply of the mixture of inert gas and fluorine. The process is carried out to equalize the concentrations of fluoride on the inlet and outlet of the reactor. Get fluorinated carbon with a bulk density of 0.01 - 0.02 g/cm3and a fluorine content of 17 to 59 wt.%. 1 C.p. f-crystals.

The invention relates to the field of chemical technology, in particular to a technology for obtaining fine powder of fluorinated carbon, used as a lubricant, thickener, smatch as cathode material in lithium chemical power sources.

A method of obtaining fine particles of fluorinated carbon by treating acetylene black gas containing fluorine at elevated temperatures (French patent, application N 2611362, publ. 02.09.88; patent Germany, application N 053805483, publ. 08.09.88; France, patent 2611362, 1987).

The methods provide fine powder of fluorinated carbon with a low bulk density 0.1 g/cm3and below. The disadvantage of these methods is the use of scarce raw materials, acetylene black, poor performance, due to the high chemical reactivity of soot.

A method of obtaining fluorinated graphite by fluorination at a temperature of 300 - 500oC subjected to swelling of graphite (Japan patent, application N 61-V, 1982). This method allows you to obtain finely dispersed fluorinated carbon with a low bulk density (less than 0.1 g/cm3). The downside of it is the need for preliminary treatment of raw carbon material (alkali metals, acids, acid salts), limited type of raw material (graphite), poor performance, due to the high chemical activity subjected to swelling of the graphite.

Svechnikova fluorine and inert gas at a temperature of 320-500oC-control process of fluoridation on the fluoride content in the gases at the inlet and outlet of the reaction zone (RF patent N 2119448, 1998 ). This method is similar to the proposed invention. It allows you to get a fluorocarbon material with a fluorine content of from 17 to 66 wt.% with a bulk density of 0.4-0.7 g/cm3.

The disadvantage of this method is the need for additional operations before using fluorinated carbon as a lubricant or lubricant compositions. The material must be atomized and to weed out the fine fraction with a particle size of about 0.1 μm with good tribological characteristics (Violet A. S. "Carbon interlayer connection and composites on its basis, Aspect press, M., 1997).

The present invention solves the problem of increasing productivity and efficiency, expanding the range of carbon source raw materials for the production of ultrafine powder of fluorinated carbon with a low bulk density (0.01 - 0.02 g/cm3).

This objective is achieved in that during production of fluorinated carbon by treating the carbon material with a mixture of technical fluorine with an inert gas at a temperature of 320 to 500oC when the control mixture cease when the ratio of the concentration of fluorine in the gas at the exit and the entrance into the reaction zone is 0.5-0.6, followed by thermal decomposition of the resulting fluorinated carbon, and the resulting thermal decomposition product is treated with a mixture of technical fluorine with an inert gas to equalize the concentrations of fluoride in the gases at the inlet and outlet of the reaction zone. Thermal decomposition can be done in different ways: by raising the temperature in the reaction zone, the flow of concentrated fluoride or air into the reaction zone. In these dangerous conditions for personnel and for equipment landslide thermal decomposition with evolution of a large quantity of gaseous fluorocarbons does not occur. All the energy released during termorasshirennyi fluorinated carbon, spent mostly on the "swelling" of the carbon material, its volume increases by about 10-20 times). This product (with a fluorine content of 11-18 wt.% ) itself suitable for use as a lubricant or lubricant compositions. Further processing of fluorine improves tribological characteristics, in particular increases the resistance. It turns out chubby fluorocarbon product with a bulk density of 0.01-0.02 g/cm3with a fluorine content of 17-65 wt.% depending on a predetermined period of fluoridation.

Below are the results of testing the method, executed on a platter Nickel ftorator with a capacity of 100 liters

Example 1

In a reactor loaded with 2 kg of carbon black - carbon black T-900. The fluorination was carried out at a temperature of 350oC with a mixture of nitrogen and technical fluoride content of fluoride in a mixture of 12%. When the concentration ratio of the fluorine gas at the outlet and the inlet of the reactor reached 0.5, stopped the flow of inert gas (nitrogen) in the reactor was applied undiluted technical fluorine (a fluorine content of 93%, HF - 3 to 5 vol.%). After 5 min occurred decomposition of fluorocarbon that recorded temperature rise in the reactor of from 350 to 420oC. the Supply of fluorine stopped and then, after lowering the temperature to 350oC, resumed feeding a mixture of nitrogen and fluorine to align fluoride concentrations at the inlet and outlet of the reactor.

Unloaded 2 kg of fluorinated at agrogene 2 kg thermoabrasion graphite. The fluorination was carried out with a mixture of fluorine with an inert gas (fluorine content of 20 vol.%) at a temperature of 500oC. At a ratio of fluoride concentrations at the outlet and the inlet of the reactor is equal to 0.6 blocked the supply of inert gas in the reactor was applied undiluted technical fluorine. After 3 minutes, there was a thermal (temperature in the reactor rose to 580oC). The supply of fluorine stopped. From the reactor was unloaded "puffy" powder with a fluorine content of 17 wt.%, bulk density of 0.01 g/cm3the mass of powder 1950

Example 3

In a reactor loaded with 2 kg thermoabrasion graphite. The fluorination was carried out with a mixture of fluorine with an inert gas (fluorine content in a mixture of 20 vol.%) at a temperature of 480oC. At a ratio of fluoride concentrations at the outlet and the inlet of the reactor is equal to 0.6 stopped feeding an inert gas. In the reactor filed undiluted technical fluorine. After 4 min, there was a thermal decomposition (leap temperature up to 600oC). The supply of fluorine stopped and after lowering the temperature to 480oC has resumed its mixture of inert gas and fluorine to align fluoride concentrations at the outlet and the inlet of the reactor.

Uploaded 1800 fluorinated carbon with a fluorine content of 59% by weight, bulk density is rather a mixture of inert gas and technical fluorine at a temperature of 320 - 500oC-control process of fluoridation on the fluoride content in the gases at the inlet and outlet of the reaction zone, wherein the fluorination process is interrupted when the ratio of the concentration of fluorine in the gas at the exit and the entrance into the reaction zone of 0.5 to 0.6, followed by the decomposition obtained fluorocarbon material and continue fluoridation thermodestruction material to equalize the concentrations of fluoride in the gases at the inlet and outlet of the reaction zone.

2. The method according to p. 1, characterized in that the decomposition of fluorinated carbon material is carried out by feeding into the reaction zone undiluted technical fluorine or air until meet a sharp increase in temperature in the reaction zone.

 

Same patents:
The invention relates to the production of ceramic, wear resistant, heat resistant and abrasive products, in particular to the field of production of raw materials for the production of these products, and can be used to obtain silicon carbide-modifications

The invention relates to the field of coordination chemistry, including physical chemistry of nanostructures and colloidal systems

The invention relates to the technique of plasma-chemical plants, in particular to devices for diamond using gas glow DC discharge at a pressure below atmospheric

The invention relates to the chemical industry and can be used to obtain acetylene
The invention relates to technologies for obtaining and purifying synthetic ultradispersed diamonds and can be used to retrieve the diamonds of detonation synthesis products

The invention relates to the field of materials science and, in particular, to obtain carbon composite materials having conductivity, which can be used in various fields of national economy, for example, for the manufacture of thin film heaters, as carriers of catalysts and adsorbents, in electrocatalysis, electrosorption, electrochemistry, etc

The invention relates to the technology for carbonitride, which is used as raw material in the production of fluorine-containing monomers

The invention relates to the production of active carbons and can be used for the heat treatment of materials in technology electro, gold extraction, construction and other industries, as well as for the reactivation of spent carbon sorbent

FIELD: carbon materials.

SUBSTANCE: invention relates to technology of manufacturing porous carbon materials based on fine-size compositions preferably for use as filter elements in micro- and ultrafiltration processes. According to invention, pore agent is dispersed via diluting it with high-dispersed carbonaceous powder in joint grinding-and-mixing process and resulting mixture is added to charge. Carbonaceous powder utilized is either carbon black or colloidal graphite with particle size not larger than 0.5 μm and pore agent-to-diluent ratio is between 1:1 and 1:2.

EFFECT: increased permeability of materials.

4 cl, 2 tbl, 2 ex

FIELD: carbon materials.

SUBSTANCE: invention concerns manufacture of diamond films that can find use in biology, medicine, and electronics. Initial powder containing superdispersed diamonds with level of incombustible residue 3.4 wt %, e.g. diamond blend, is placed into quartz reactor and subjected to heat treatment at 600-900оС in inert of reductive gas medium for 30 min. When carbon-containing reductive gas medium is used, heat treatment is conducted until mass of powder rises not higher than by 30%. After heat treatment, acid treatment and elevated temperatures is applied. Heat treatment and acid treatment can be repeated several times in alternate mode. Treated powder is washed and dried. Level of incombustible impurities is thus reduced to 0.55-0.81 wt %.

EFFECT: reduced level of incombustible impurities.

4 cl, 3 ex

FIELD: carbon materials.

SUBSTANCE: weighed quantity of diamonds with average particle size 4 nm are placed into press mold and compacted into tablet. Tablet is then placed into vacuum chamber as target. The latter is evacuated and after introduction of cushion gas, target is cooled to -100оС and kept until its mass increases by a factor of 2-4. Direct voltage is then applied to electrodes of vacuum chamber and target is exposed to pulse laser emission with power providing heating of particles not higher than 900оС. Atomized target material form microfibers between electrodes. In order to reduce fragility of microfibers, vapors of nonionic-type polymer, e.g. polyvinyl alcohol, polyvinylbutyral or polyacrylamide, are added into chamber to pressure 10-2 to 10-4 gauge atm immediately after laser irradiation. Resulting microfibers have diamond structure and content of non-diamond phase therein does not exceed 6.22%.

EFFECT: increased proportion of diamond structure in product and increased its storage stability.

2 cl

FIELD: nonferrous metallurgy.

SUBSTANCE: invention relates to hydrometallurgy of rare-earth elements, in particular to technology of preparing of rare-earth element carbonates with controlled particular shape used in manufacture of polishing materials and catalysts. Suspension of rare-earth element carbonates prepared by mixing rare-earth element carbonate solution with carbonic acid solution is stirred at 20 to 75оС at suspension motion velocity between 0.5 and 20 m/s, whereupon rare-earth element carbonates are precipitate in plate form at stirring for a period of time satisfying relationship 1.5*T0.5 ≤ τ ≤ 30. Precipitation of dendritic carbonates is accomplished at stirring for a period of time satisfying relationship 106*T-2.5 ≤ τ ≤ 600, where τ are numeric values of stirring time, min, and T are numeric values of reaction medium temperature, оС.

EFFECT: extended temperature range for precipitation of plate- and dendritic-form rare-earth element carbonates and improved granulometric uniformity of product.

2 dwg, 2 ex

FIELD: non-iron industry.

SUBSTANCE: invention relates to method for reducing of manganese oxide from ore to manganese carbide. Solid metal oxide is brought into contact with gaseous reducing and cementation agent (e.g., hydrogen-hydrocarbon mixture), and optionally, with inert gas at temperature of 1000-12500C.

EFFECT: environmentally friendly method; decreased energy consumption.

21 cl, 22 dwg, 1 tbl

FIELD: production of charcoal-fibrous adsorbents.

SUBSTANCE: the invention is dealt with the field of production of charcoal-fibrous adsorbents, in particular, with devices of charcoal-fibrous materials activation. The installation contains a vertical furnace for activation of a carbon fabric and a conjugated with it steam generator, which are connected to the power source and a control unit. And at the furnace output there is a reception device. At that the furnace contains a through heated muffle, through which the treated charcoal-fibrous fabric is continuously passing. At that the muffle is located inside the detachable heat-insulating furnace body, on the inner side of which there are heating elements. Besides at the furnace outlet there is a movable container with water, in which the lower end of the through muffle is dipped. The invention offers an installation for production of activated charcoal-fibrous material, which ensures a continuous process of treatment of the charcoal-fibrous material with an overheated steam and formation of the activated fabric with high mechanical properties and a cellular structure, simple in assembly and reliable in operation.

EFFECT: the invention ensures production of the activated fabric with high mechanical properties and a cellular structure, simple in assembly and reliable in operation.

8 cl, 4 dwg

FIELD: sorption technique for purification of industrial emissions and individual pipe security facilities.

SUBSTANCE: method for production of sorbent catalyst includes preparation of impregnating solution by introducing ammonium carbonate and copper and chromium compounds into ammonia water in ratio ammonia water/ammonium carbonate/copper basic carbonate/chrome anhydride of 1:(0.07-0.15):(0.03-0.06):(0.02-0.04); impregnation with metal-containing carbon solution; aging; and granule thermal treatment.

EFFECT: sorbent catalyst with prolonged protective action in relation to chlorocyanide and decreased cost.

4 cl, 3 ex

FIELD: selective oxidation of carbon monoxide in hydrogen-containing stream.

SUBSTANCE: invention relates to method for selective oxidation of carbon monoxide to carbon dioxide in raw material containing hydrogen and carbon monoxide in presence of catalyst comprising platinum and iron. Catalyst may be treated with acid. Certain amount of free oxygen is blended with mixture containing hydrogen and carbon monoxide to provide second gaseous mixture having elevated ratio of oxygen/carbon monoxide. Second gaseous mixture is brought into contact with catalyst, containing substrate impregnated with platinum and iron. Carbon monoxide in the second gaseous mixture is almost fully converted to carbon dioxide, i.e. amount of carbon monoxide in product stream introduced into combustion cell is enough small and doesn't impact on catalyst operation characteristics.

EFFECT: production of hydrogen fuel for combustion cell with industrial advantages.

13 cl, 1 tbl, 4 ex

FIELD: chemical industry and electronics; production of diamonds.

SUBSTANCE: the invention is intended for chemical industry and electronics. The chemical product is prepared out of the following organic compounds (in weight %): acetamide - 6.7; carbamide - 0.8; ethylene glycol - 2.0; glycolic acid - 11.7; lactamide - 8.8; glycerine - 2.3; hexamethylenetetramine - 11; indene - 7.6; 1,2-dimethylnaftaline - 2.6; 1,4 -diisopropenylbenzol - 3.3; cyclohexylphenylketon - 8.1; 4'-cyclohexylacetophenone - 7.2; 4-(1-adamantyl)phenol - 2.1; 4,4'-methylenebis (2,6-dimethyl phenol) - 2.3; α,α'- bis (4-hydroxyfenyl)-1.4-diisopropylbenzol - 0.2; phenanthrene - 11.0; lauric acid - 6.2; sebacic acid-6.3; eicosanic acid - 9.7. The indicated components are mixed with water in the ratio of 1:(1-2). The mixture is heated up to 150-200°С in vacuum of 10-1-10-6Pa. A reaction sample formed this way is refrigerated in conditions of vacuum and dried for removal of water and the volatile organic substances. The dried reaction sample is heated in vacuum up to 200-400°С for 80 hours. The invention allows to use the raw material being in lower power state as compared with the known methods and to produce the high-clean diamonds.

EFFECT: the invention ensures production of the high-clean diamonds from the raw material of the lower power state.

16 cl, 1 tbl, 1 ex, 4 dwg

FIELD: production of color diamonds.

SUBSTANCE: the invention is pertaining to the field of production of fantasy neon yellow-green diamonds of precious quality produced from the pale (discolored) or so-called "brown" diamonds of the lowest quality. The method provides for placement of a pale natural diamond in the medium capable to transfer the pressure, which then is mold into a "tablet". Then the tablet is placed in the high-pressure press (HP/HT) and exposed to machining at an increased pressure and temperature being within the range of graphite stability or a diamond being on the phase diagram of carbon for the period of time necessary for improvement of a color of the mentioned diamond. In the end the diamond is removed from press. The indicated method ensures production of diamonds of an attractive yellowish-green or yellow-green and neon yellow-green colors.

EFFECT: the invention ensures production of diamonds of attractive yellow-green colors.

22 cl, 4 ex, 2 dwg

Up!