CN109704325B - Method for extracting flaky graphitized carbon body in human hair by taking transition metal alloy as catalyst - Google Patents
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Abstract
A method for extracting flaky graphitized carbon body from human hair by using transition metal alloy as a catalyst. The invention discloses a process for extracting high-purity and high-graphitization carbon from human hair, which comprises the steps of taking human hair as an initial raw material, carrying out primary treatment on the hair, roasting, adding a binder, carrying out compression molding, taking the obtained product as a reaction raw material, using an alloy of transition metals such as iron, cobalt, nickel, manganese and the like as a catalyst, and obtaining high-purity flaky graphite by utilizing a concentration gradient diffusion principle under the conditions of high temperature and high pressure. The method can extract high-purity and high-graphitization-degree carbon from human hair, and has the advantages that strong acid and strong alkali are not used in the process of extracting the graphitization carbon from the human hair, so that the pollution to the environment is reduced. Due to the use of the metal catalyst, high graphitization of carbon is achieved at lower temperatures. The obtained flaky graphitized carbon can meet the requirements of large diamond single crystals or industrial diamond abrasive materials cultured by an artificial high-temperature high-pressure method on carbon source purity and graphitization degree, and can also be used as an initial reaction raw material of graphene.
Description
Technical Field
The invention relates to a preparation method of a graphitized carbon body, in particular to a method for extracting a scale-shaped graphitized carbon body in human hair by taking a transition metal alloy as a catalyst.
Background
The human hair is mainly composed of keratin, and compared with other biological materials, the carbon content in the human hair is higher and can reach 45.2%. The extraction of high-purity and high-graphitization-degree carbon bodies from human hair has been a technical problem accepted by the scientific community, and the main difficulty is that biomass carbon belongs to carbon bodies difficult to graphitize, even after a plurality of times of physicochemical purification, the purity can reach very high and can reach 98% -99% (such as patent WO2009091285A1), but the biomass carbon is difficult to completely graphitize, only partial graphite phase can be generated even under the high-temperature environment of 2500-3000 ℃, and the graphitization process is very slow. It is reported that the graphitization temperature can be lowered by adding a metal element such as silicon iron, titanium, or aluminum to carbon that is difficult to graphitize, but it is also difficult to obtain a graphitized carbonaceous body of 99% or more. In addition, the graphite phase in the carbonaceous body obtained by this method is spherical graphite, not flake graphite. Therefore, how to effectively extract the high-purity and high-graphitization-degree flaky graphite from the human hair is not well solved all the time.
Disclosure of Invention
In view of the above, the present invention provides a method for effectively extracting high-purity and high-graphitization scale-like carbon body from human hair, wherein the purity can reach 99.99%, the graphitization degree can reach 99.99%, and the scale-like carbon body has the same atomic structure, the same form, the similar density and the same conductivity as natural scale graphite.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for extracting flaky graphitized carbon bodies in human hair by taking transition metal alloy as a catalyst comprises the following steps:
(1) cleaning and drying human hair, placing the human hair into an alumina container, placing the human hair into an atmosphere sintering furnace for roasting, and continuously feeding fresh air, wherein the roasting temperature is 350-;
(2) placing the primary sintered product of the organic biochar in an alumina ceramic container, and roasting in a vacuum tube furnace under the conditions of negative pressure of 0.08-0.1MPa, temperature of 1300 ℃ and 1400 ℃, heating rate of 2-5.5 ℃/min and roasting time of 2-5h to obtain biomass carbon body powder;
(3) ball-milling a biomass carbon body by using a planetary ball mill, wherein the ball-milling medium is tungsten carbide balls, the ball-milling tank is made of stainless steel, the ball-milling condition is 800-;
(4) pressing the biological carbon powder into blocks, roasting again in a high-temperature tubular vacuum furnace under the conditions of negative pressure of 0.08-0.1MPa, temperature of 900-;
placing a cylindrical carbon body in an assembly block, adding a metal catalyst, pressurizing and heating the assembly block, heating the assembly block to 4-5GPa, 1400 ℃ and 1600 ℃, keeping the pressure and the temperature for 24-72 hours, releasing the pressure to 1 atmosphere after stopping heating, taking out the assembly block for crushing, and taking out a metal block body containing flaky graphite;
(5) carrying out acid washing separation on the flaky graphite and the metal, heating and distilling at 90-110 ℃ until no bubbles are generated, and filtering to obtain a highly graphitized carbon body;
(6) crushing the highly graphitized carbon body, then carrying out acid washing again until no bubbles are generated, filtering, and then repeatedly washing with clear water to finally obtain graphitized carbon powder;
(7) ultrasonically cleaning and drying the graphitized carbon powder to obtain the flaky graphitized carbon body;
the metal catalyst is a bulk alloy of a transition metal.
In the prior art, when a metal catalyst is used for catalyzing biochar or graphitized carbon, the commonly used catalyst is powdered materials such as iron silicide, metal titanium, aluminum and the like, the metal powder is usually mixed with biomass carbon or a carbon body which is difficult to graphitize, and then high-temperature graphitization catalysis is carried out under the condition of no pressure or low pressure, the graphitization degree of the obtained graphitized carbon body is low, and the obtained carbon body is spherical powder, but the method for extracting the flaky graphitized carbon body in the human hair by using the bulk alloy of transition metal as the catalyst fully considers the problem of environmental pollution in the process of extracting graphitized carbon from the human hair, does not use strong acid and strong alkali solution, does not use reducing gas and oxidizing gas, only uses a certain amount of dilute nitric acid solution, and greatly reduces the environmental pollution, during high-temperature high-pressure catalysis, a transition metal catalyst is used as a catalytic medium, so that the catalytic condition is greatly reduced, compared with the condition without the catalyst, the graphitization temperature is reduced by 1000 ℃, the transition metal catalytic medium is made of a block material instead of a powder material, the transition metal catalytic medium is heated to a temperature higher than the melting point temperature under the extreme pressure of 4-5GPa to reach a molten state, biochar is fully dissolved and then separated out, the separation out process essentially realizes the process of rearranging carbon atoms, and the separated out carbon has the same physical and chemical properties as natural flake graphite.
Further, tail gas in the roasting process in the step (1) is discharged into a water tank.
Adopt above-mentioned further beneficial effect to lie in, the tail gas is discharged after water filters, prevents the pollution of combustion gas to the environment.
Further, in the step (3), the solvent is one or more of saturated phenolic resin alcohol solution and acetone solution, and the adding amount is 4-10 times of the mass of the biological carbon body.
The further beneficial effect is that the saturated phenolic resin alcohol solution and the acetone solution are used as the solvent to contribute to the powder particle forming.
Further, the bulk alloy of the transition metal is an alloy prepared by mixing two or more of iron, cobalt, nickel and manganese in any ratio, the addition amount is 10-50g, and preferably the weight ratio of nickel, manganese and cobalt is 75: 25:5, and the addition amount of the alloy is 10-50 g.
The further beneficial effects of the adoption of the method are that the catalytic activity of cobalt and nickel is high, the alloy prepared by matching manganese in a specific ratio can further greatly reduce the catalytic condition, compared with the condition without a catalyst, the graphitization temperature is reduced by 1000 ℃, the separated carbon has the same physical and chemical properties with natural flake graphite, the separation of the catalyst and the graphitized carbon body in the later period is very easy, only dilute nitric acid is needed for soaking, an electric furnace is not needed for heating, and the energy consumption is lowest.
Further, the condition of catalyzing carbon deposition in the step (4) is that the catalyzing time is set according to the amount of the catalyzing hair at the temperature of 1400 ℃ and 1600 ℃ and the pressure of 4.0-5.0GPa, and is usually 24-72 h.
The method has the further beneficial effects that under the conditions of high temperature and high pressure, the concentration gradient diffusion principle is utilized, the biomass carbon body is placed at the high-temperature end of the assembly block, the metal catalyst is placed at the low-temperature end, the carbon dissolved in the catalyst is diffused from the high-temperature end to the low-temperature end under the drive of the concentration gradient, and is crystallized and separated out at the low-temperature end in a graphite state form, so that the conversion of the carbon from an amorphous state to a crystalline state is completed, the scaly graphite is obtained, strong acid, strong alkali solution, reducing gas and oxidizing gas are not required, and the pollution to the environment is greatly reduced.
Further, the assembly block comprises a pressure transmission medium pyrophyllite, a dolomite heat preservation ring, a sodium chloride ring, a graphite heating pipe, an alumina plug, a magnesia plug ring, a conductive electrode and a zirconia plug ring,
openings are formed in the upper side and the lower side of the pressure transfer medium pyrophyllite and penetrate through the pressure transfer medium pyrophyllite to form a cavity channel, the openings at the two ends of the pressure transfer medium pyrophyllite are sealed by conductive electrodes to form a reaction chamber, a graphite heating pipe is arranged in the reaction chamber, the upper end and the lower end of the graphite heating pipe are abutted against the conductive electrodes, a cavity is formed in the graphite heating pipe, the cavity is internally provided with alumina plug-coated re-roasted biological carbon powder and a metal catalyst, and the re-roasted biological carbon powder is located above the metal catalyst and is in close contact with the metal; a dolomite heat preservation ring, a sodium chloride ring and a zirconia plugging ring are sequentially arranged between the pressure transfer medium pyrophyllite and the graphite heating pipe, and the vacant position of the reaction chamber is filled with the magnesia plugging ring for fixing the graphite heating pipe.
The structure is different from the assembly used for cultivating diamond by a temperature gradient method under the conditions of high temperature and high pressure, the inner part of the assembly block has a larger temperature gradient, the temperature gradient is set to be 5-8 ℃/mm, and the crystallization rate of the carbon body in the metal catalyst is controlled to be 30-80 mg/h. In addition, the assembled design can be stably maintained for 72 hours under the high-temperature condition of 1600 ℃.
Further, the pickling is performed with a 20 to 37% nitric acid solution, and preferably with a 37% nitric acid solution.
The further beneficial effect of the method is that the metal catalyst and other impurities can be effectively removed by acid washing with 20-37% dilute nitric acid.
Further, the ultrasonic cleaning operation in the step (7) is as follows: and soaking the graphitized carbon powder in absolute ethyl alcohol, and carrying out ultrasonic cleaning for 10-30min at the frequency of 30-40 kHz.
The further beneficial effects of the method are that the residual acid liquor can be effectively removed, and the purity of the graphitized carbon body can be ensured.
Drawings
FIG. 1 is a cross-sectional view of the assembly block structure of the present invention;
FIG. 2 is an XRD diffraction pattern of the flaky graphitized carbosome prepared in example 1 of the present invention;
fig. 3 is an XRD diffraction pattern of the flaky graphitized carbosome prepared in example 2 of the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
101, pressure transmission medium pyrophyllite; 102, a dolomite thermal insulation ring; 103, sodium chloride ring; 104, graphite heating pipes; 105, alumina plugs; 106, magnesium oxide blocking ring; 107, a conductive electrode; and 108, blocking the ring by using zirconium oxide.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the structure of the assembly block is shown in fig. 1, the assembly block comprises a pressure transmission medium pyrophyllite 101, a dolomite thermal insulation ring 102, a sodium chloride ring 103, a graphite heating pipe 104, an alumina plug 105, a magnesia plug 106, a conductive electrode 107 and a zirconia plug 108,
openings are formed in the upper side and the lower side of the pressure transfer medium pyrophyllite 101 and penetrate through the pressure transfer medium pyrophyllite 101 to form a cavity channel, the openings at the two ends of the pressure transfer medium pyrophyllite 101 are sealed by conductive electrodes 107 to form a reaction chamber, a graphite heating pipe 104 is arranged in the reaction chamber, the upper end and the lower end of the graphite heating pipe 104 are abutted to the conductive electrodes 107, a cavity is formed in the graphite heating pipe 104, the cavity is internally provided with calcined biological carbon powder and a metal catalyst which are coated by an aluminum oxide plug 105, and the calcined biological carbon powder is located above the metal catalyst and is in close contact with the metal; a dolomite heat preservation ring 102, a sodium chloride ring 103 and a zirconia plugging ring 108 are sequentially arranged between the pressure transmission medium pyrophyllite 101 and the graphite heating pipe 104, and a magnesium oxide plugging ring 106 for fixing the graphite heating pipe 104 is filled in the vacant position of the reaction chamber.
Other instruments or reagents not specifically described are conventional instruments or reagents available from the existing sources.
Example 1
(1) Soaking 50g of human hair into 95% alcohol, performing ultrasonic cleaning, placing the human hair in a drying oven at 100 ℃ for 1h to dry water, then placing the human hair in an alumina crucible, placing the alumina crucible in an atmosphere sintering furnace for roasting, continuously feeding fresh air, wherein the roasting temperature is 370 ℃, the heating rate is 6 ℃/min, and the roasting time is 2h, so as to obtain a primary roasted product of organic biochar;
(2) placing the primary burned product of the organic biochar in an alumina ceramic burning boat, and roasting in a vacuum tube furnace under the conditions of negative pressure of 0.08MPa, temperature of 1400 ℃, heating rate of 5.5 ℃/min and roasting time of 2h to obtain a biomass carbon body;
(3) ball-milling a biomass carbon body by using a planetary ball mill, wherein a ball-milling medium is tungsten carbide balls, a ball-milling tank is made of stainless steel, the ball-milling condition is 1000r/min, the time is 1h, then adding an alcohol solution in which phenolic resin is dissolved, the adding amount is 10 times of the mass of the biomass carbon body, the content of the phenolic resin accounts for 20% of the mass of the biocarbon, fully stirring, placing on a heating furnace for drying, the drying time is 1h, and then ball-milling the biocarbon again to obtain biocarbon powder;
(4) pressing biological carbon powder into blocks, roasting again in a high-temperature tubular vacuum furnace under the conditions of negative pressure of 0.08MPa, temperature of 900 ℃, heating rate of 5.5 ℃/min, keeping the temperature for 3h, and roasting to obtain cylindrical carbon bodies;
placing the carbon body in an assembly block, the assembly mode of the assembly block is shown in figure 1, and the size of the assembly block is 42 x 42mm3The diameter of an inner cavity of the assembly block is 17mm, cylindrical nickel-cobalt alloy is placed at the lower end of a carbon body, the mass ratio of nickel to cobalt in the nickel-cobalt alloy is 1:1, the mass of the nickel-cobalt alloy is 10g, the assembly block is placed in phi 420 cubic press equipment for heating and pressurizing, the temperature is increased to 1500 ℃, the pressure is increased to 4GPa, the heat is stopped after the assembly block is kept for 36h, the pressure is released to a standard atmospheric pressure, the assembly block is crushed, and gold containing graphite is taken outBelongs to a block body.
(5) Carrying out acid washing separation on the flake graphite and the metallic iron by 37% nitric acid solution, heating and distilling at 90 ℃ until no bubbles are generated, and filtering acid liquor to obtain highly graphitized carbon body;
(6) crushing the highly graphitized carbon body, then pickling with 37% nitric acid solution again until no bubbles are generated, filtering, and then adding clear water to wash for 3 times to finally obtain graphitized carbon powder;
(7) and ultrasonically cleaning the graphitized carbon powder at the frequency of 30kHz for 30 minutes, and drying the graphitized carbon powder in a drying box at the temperature of 120 ℃ for 1 hour to obtain the flaky graphitized carbon body with the mass of about 3.5g, wherein an XRD diffraction pattern is shown as a figure 2, the diffraction pattern has a complete set of graphite diffraction peaks, and no diffraction peaks of other impurity elements are found, which indicates that the purity of the carbon is very high.
Example 2
(1) Soaking 80g of human hair into 95% alcohol, performing ultrasonic cleaning, placing the human hair in a drying oven at 120 ℃ for 1h to dry water, then placing the human hair in an alumina crucible, placing the alumina crucible in an atmosphere sintering furnace for roasting, and continuously feeding fresh air, wherein the roasting temperature is 350 ℃, the heating rate is 6 ℃/min, and the roasting time is 3h, so as to obtain a primary roasted product of organic biochar;
(2) placing the obtained primary burned product of the organic biochar in an alumina ceramic container, and roasting in a vacuum tube furnace under the conditions of negative pressure of 0.1MPa, temperature of 1300 ℃, heating rate of 5.5 ℃/min and roasting time of 5h to obtain a biomass carbon body;
(3) ball-milling a biomass carbon body by using a planetary ball mill, wherein ball-milling media are zirconia balls, a ball-milling tank is made of agate materials, the ball-milling condition is 800r/min, the time is 2 hours, then adding an absolute alcohol solution dissolved with phenolic resin, the adding amount is 6 times of the mass of the biomass carbon body, the content of the phenolic resin accounts for 20 percent of the content of the biocarbon, fully stirring, placing on a heating furnace for drying, drying for 1 hour, and ball-milling and crushing again to obtain biocarbon powder;
(4) pressing the biological carbon powder into blocks, roasting again in a high-temperature tubular vacuum furnace under the conditions of negative pressure of 0.08MPa, temperature of 1000 ℃, heating rate of 5.5 ℃/min and heat preservation for 3h to obtain cylindrical carbon bodies;
placing the carbon body in an assembly block, the assembly mode of the assembly block is shown in figure 1, and the size of the assembly block is 64 x 64mm3And the diameter of an inner cavity of the assembly block is 32mm, a cylindrical nickel-manganese-cobalt alloy is placed at the lower end of the carbon element to be catalyzed, and the weight ratio of nickel to manganese to cobalt in the nickel-manganese-cobalt alloy is 75: 25:5, the mass of the nickel-manganese-cobalt alloy is 30g, the nickel-manganese-cobalt alloy is used for catalytic graphitization, the assembly block is placed in a phi 650 cubic press, the assembly block is heated and pressurized, the temperature is increased to 1400 ℃, the pressure is increased to 4GPa, the heat is stopped after the temperature is maintained for 72h, the pressure is released to a standard atmospheric pressure, and the assembly block is crushed to take out the metal block containing graphite.
(5) Pickling and separating the flake graphite by using a 20% nitric acid solution, heating and distilling at 100 ℃ until no bubbles are generated, filtering acid liquor, washing the carbon body for 5 times by using clear water, and filtering water to obtain the highly graphitized carbon body;
(6) crushing the highly graphitized carbon body, then pickling with 37% nitric acid solution again until no bubbles are generated, filtering, and washing the flake graphite with clear water to obtain a flake graphitized carbon body finally;
(7) and ultrasonically cleaning the graphitized carbon powder at the frequency of 30kHz for 30 minutes, and drying in a drying box at the temperature of 120 ℃ for 1 hour to obtain the flaky graphitized carbon body with the mass of about 6g, wherein an XRD diffraction pattern is shown as a figure 3, the diffraction pattern has a complete set of graphite diffraction peaks, no diffraction peaks of other impurity elements are seen, and the purity of the carbon is very high.
Example 3
(1) Soaking 100g of human hair into 95% alcohol, performing ultrasonic cleaning, placing the human hair in a drying oven at 120 ℃ for 1h to dry water, then placing the human hair in an alumina crucible, placing the alumina crucible in an atmosphere sintering furnace for roasting, and continuously feeding fresh air, wherein the roasting temperature is 360 ℃, the heating rate is 5 ℃/min, and the roasting time is 3h, so as to obtain a primary roasted product of organic biochar;
(2) placing the primary burned product of the organic biochar in an alumina ceramic container, and roasting in a vacuum tube furnace under the conditions of negative pressure of 0.1MPa, temperature of 1350 ℃, heating rate of 5 ℃/min and roasting time of 5h to obtain a biomass carbon body;
(3) ball-milling a biomass carbon body by using a planetary ball mill, wherein ball-milling media are zirconia balls, a ball-milling tank is made of agate materials, the ball-milling condition is 1200r/min, the time is 0.5h, then adding acetone solution dissolved with phenolic resin, the adding amount is 10 times of the mass of the biomass carbon body, the content of the phenolic resin accounts for 20 percent of the content of the biochar, drying for 1h by using an electric furnace after fully stirring, and ball-milling and crushing again to obtain biochar powder;
(4) pressing the biological carbon powder into blocks, roasting again in a high-temperature tubular vacuum furnace under the conditions of negative pressure of 0.1MPa, temperature of 900 ℃, heating rate of 5.5 ℃/min and heat preservation for 3h to obtain cylindrical graphitized carbon bodies;
placing the carbon body in an assembly block, the assembly mode of the assembly block is shown in figure 1, and the size of the assembly block is 76 × 76mm3The diameter of the inner cavity of the assembly block is 41mm, the lower end of the carbon element is placed with a cylindrical iron-cobalt-nickel alloy, and the weight ratio of iron to cobalt to nickel in the iron-cobalt-nickel alloy is 80: 20:15, the mass of the iron-cobalt-nickel alloy is 50g, the iron-cobalt-nickel alloy is used for catalyzing graphitization, the assembly block is placed in a phi 750 cubic press, the assembly block is heated and pressurized, the temperature is increased to 1400 ℃, the pressure is increased to 4GPa, the heat is stopped after the temperature is maintained for 72h, the pressure is released to a standard atmospheric pressure, and the assembly block is crushed to take out the metal block containing graphite.
(5) Pickling and separating the flaky graphite and the metallic cobalt by using a 20% nitric acid solution, heating and distilling at 100 ℃ until no bubbles are generated, filtering acid liquor, washing the carbon body for 5 times by using clear water, and filtering water to obtain the highly graphitized carbon body;
(6) and crushing the highly graphitized carbon body, then pickling with 20% nitric acid solution again until no bubbles are generated, and washing the flake graphite with clear water to obtain the flake graphitized carbon body.
(7) And ultrasonically cleaning the graphitized carbon powder at the frequency of 40kHz for 30min, and drying the graphitized carbon powder in a drying box at the temperature of 120 ℃ for 1 hour to obtain the flaky graphitized carbon body with the mass of about 7.5 g.
Claims (8)
1. A method for extracting flaky graphitized carbon bodies in human hair by taking transition metal alloy as a catalyst is characterized by comprising the following steps:
(1) cleaning and drying human hair, putting the human hair into an alumina container, putting the aluminum container into an atmosphere sintering furnace for roasting, and continuously feeding fresh air to obtain a primary burnt product of organic biochar;
(2) placing the primary burned product of the organic biochar in an alumina ceramic container, and roasting in a vacuum tube furnace to obtain a biomass carbon body;
(3) adding a solvent into the biomass carbon body after ball milling, fully stirring, drying, and performing ball milling and crushing again to obtain biological carbon powder;
(4) pressing the biochar powder into blocks, roasting again in a high-temperature tubular vacuum furnace, adding a metal catalyst, placing the blocks in an assembly block for catalyzing carbon deposition, heating and pressurizing the assembly block, and catalyzing biochar by using transition metal;
(5) carrying out acid washing separation on the flaky graphite, heating and distilling until no bubbles are generated, and filtering to obtain a highly graphitized carbon body;
(6) crushing the highly graphitized carbon body, then pickling again until no bubbles are generated, filtering out acid liquor, then repeatedly cleaning with clear water, and finally filtering out water to obtain the graphitized carbon body;
(7) ultrasonically cleaning and drying the graphitized carbon powder to obtain the flaky graphitized carbon body;
in the step (4), the metal catalyst is a bulk alloy of transition metal; the bulk alloy of the transition metal is an alloy of two or more of iron, cobalt and manganese, and the addition amount is 10-50 g;
the roasting condition is that the negative pressure is 0.08-0.1MPa, the temperature is 900-;
the conditions of the catalytic carbon deposition are 1400-1600 ℃, the pressure is 4.0-5.0GPa, and the deposition time is 24-72 h;
the assembly block comprises a pressure transmission medium pyrophyllite (101), a dolomite heat preservation ring (102), a sodium chloride ring (103), a graphite heating pipe (104), an alumina plug (105), a magnesia plug ring (106), a conductive electrode (107) and a zirconia plug ring (108), openings are arranged on the upper side and the lower side of the pressure transmission medium pyrophyllite (101) and penetrate through the pressure transmission medium pyrophyllite (101) to form a cavity, the openings at the two ends of the pressure transmission medium pyrophyllite (101) are sealed by the conductive electrodes (107) to form a reaction chamber, the graphite heating pipe (104) is arranged in the reaction chamber, the upper end and the lower end of the graphite heating pipe (104) are abutted against the conductive electrode (107), a cavity is arranged in the graphite heating pipe (104), the cavity is internally provided with the calcined biological carbon powder and the metal catalyst which are coated by the alumina plug (105), and the calcined biological carbon powder is positioned above the metal catalyst and is in close contact with the metal catalyst; the dolomite insulation ring (102), the sodium chloride ring (103) and the zirconia plugging ring (108) are sequentially arranged between the pressure transmission medium pyrophyllite (101) and the graphite heating pipe (104), and the magnesia plugging ring (106) for fixing the graphite heating pipe (104) is filled in the vacant position of the reaction chamber.
2. The method for extracting flaky graphitized carbon body in human hair with transition metal alloy as catalyst in claim 1, wherein the calcination temperature in step (1) is 350-370 ℃, the temperature rise rate is 2-6 ℃/min, and the calcination time is 2-5 h.
3. The method for extracting flaky graphitized carbon body in human hair with transition metal alloy as catalyst in claim 1, wherein the calcination condition in step (2) is 0.08-0.1MPa of negative pressure, 1300 ℃ and 1400 ℃, 2-5.5 ℃/min of temperature rise rate and 2-5h of time.
4. The method for extracting flaky graphitized carbon bodies in human hair by using transition metal alloy as a catalyst in claim 1, wherein the ball milling operation in step (3) is ball milling by using a ball mill, and the ball milling condition is 800-.
5. The method for extracting flaky graphitized carbon bodies in human hair by using transition metal alloy as a catalyst in claim 1, wherein the solvent in step (3) is one or more of saturated phenolic resin alcoholic solution and acetone solution, and the addition amount is 4-10 times of the mass of the biochar.
6. The method for extracting flaky graphitized carbosome in human hair by using transition metal alloy as a catalyst in claim 1, wherein the acid washing in the step (5) is performed by using 20% -37% nitric acid solution; the temperature of the heating distillation is 90-110 ℃.
7. The method for extracting flaky graphitized carbosome in human hair by using transition metal alloy as a catalyst in claim 1, wherein the acid washing in the step (6) is performed by using 20% -37% nitric acid solution.
8. The method for extracting flaky graphitized carbosome in human hair by using transition metal alloy as a catalyst in claim 1, wherein the operation of ultrasonic cleaning in step (7) is as follows: and soaking the graphitized carbon powder in absolute ethyl alcohol, and carrying out ultrasonic cleaning for 10-30min at the frequency of 30-40 kHz.
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