CN109796207A - One kind extracting flaky graphite carbon body method in human hair by catalyst of transition metal simple substance - Google Patents

One kind extracting flaky graphite carbon body method in human hair by catalyst of transition metal simple substance Download PDF

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CN109796207A
CN109796207A CN201910049366.0A CN201910049366A CN109796207A CN 109796207 A CN109796207 A CN 109796207A CN 201910049366 A CN201910049366 A CN 201910049366A CN 109796207 A CN109796207 A CN 109796207A
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carbon
human hair
transition metal
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flaky graphite
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CN109796207B (en
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叶克晓
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Zhejiang Jianshang Technology Co Ltd
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Abstract

The invention discloses a kind of to extract high-purity, the technique of high graphitization degree carbon from human hair, initial feed has drawn from the hair of human body, by to hair preliminary treatment, roasting, binder compression moulding is added and uses the elemental metals such as iron, cobalt, nickel, manganese as catalyst as reaction raw materials, concentration gradient diffusion principle is utilized under high-temperature and high-pressure conditions, obtains the flaky graphite of high-purity.The present invention can extract high-purity, high graphitization degree carbon from human hair, it is advantageous that not using strong acid and strong base during extracting graphitized carbon from human hair, reduce the pollution to environment.Due to the use of metallic catalyst, the high-graphitized of carbon is realized at a lower temperature.Obtained flaky graphite carbon can satisfy artificial high temperature and high pressure method and cultivate the requirement of gem grade diamond large single crystal or structure bort abrasive material to carbon source purity and degree of graphitization, can also be used as the initial reaction raw material of graphene.

Description

One kind extracting flaky graphite in human hair by catalyst of transition metal simple substance Carbon body method
Technical field
The present invention relates to the preparation methods of graphitized carbon ferritic, and in particular to one kind is mentioned using transition metal simple substance as catalyst Take flaky graphite carbon body method in human hair.
Background technique
Human hair is mainly made of keratin, compares other organisms material, and the carbon content in human hair is higher It can reach 45.2%.All the time, high-purity is extracted from human hair, the carbon body of high graphitization degree is scientific circles' public affairs always The technical problem recognized, Major Difficulties are that biomass carbon belongs to and are difficult to graphited carbon body, even if by multiple physical chemistry After purification, purity can reach very high, can reach 98%-99% (such as patent WO2009091285A1), but be also difficult by It is graphitized completely, even if can only generate part graphite-phase, and be graphitized under 2500 DEG C -3000 DEG C of hot environment Cheng Shifen is slow.It is reported that graphite can be reduced by adding the metallic elements such as ferrosilicon, titanium, aluminium in being difficult to graphited carbon Changeization temperature, but also hardly result in 99% or more graphitized carbon ferritic.Furthermore the graphite in carbon body that this method obtains It is mutually globular graphite, rather than flaky graphite.Therefore how high-purity, high graphitization degree are effectively extracted from human hair Flaky graphite always without very good solution.
Summary of the invention
In view of this, the present invention provides the squamas that one kind can effectively take high-purity, high graphitization degree from human hair The method of sheet carbon body, purity can reach 99.99%, and degree of graphitization can reach 99.99%, have and natural scale stone The identical atomic structure of ink, identical form, similar density, identical conductivity.
To achieve the goals above, the present invention adopts the following technical scheme:
One kind using transition metal simple substance as catalyst extract human hair in flaky graphite carbon body method, including with Lower step:
(1) it is put into alumina container after human hair being cleaned drying, is placed in atmosphere sintering furnace and is roasted and held Continuous to be sent into fresh air, the temperature of roasting is 350-370 DEG C, and 2-6 DEG C of heating rate/min, calcining time 2-5h is had The first burning product of machine matter biological carbon;
(2) the first burning product for obtaining Organic biological carbon are held with aluminium oxide ceramics container, is placed in vacuum tube furnace It is roasted, the condition of roasting is negative pressure 0.08-0.1MPa, and temperature is 1300-1400 DEG C, 2-5.5 DEG C of heating rate/min, roasting The burning time is 2-5h, obtains biomass carbon ferritic powder;
(3) biomass carbon ferritic is subjected to ball milling with planetary ball mill, ball-milling medium is tungsten-carbide ball, and ball grinder is stainless Solvent is then added in steel material, ball milling condition 800-2000r/min, time 0.5-2h, dries after being sufficiently stirred, again ball It is milled broken, obtains biological carbon dust;
(4) it by biological carbon dust briquet shape, is roasted again in high-temperature tubular vacuum drying oven, roasting condition is negative pressure 0.08-0.1MPa, 900-1200 DEG C of temperature, 2-5.5 DEG C of heating rate/min keeps the temperature 2-5h, obtains cylindric carbon body;
Cylindric carbon body is placed in assembling block, metallic catalyst is added, and pressurized, heated, pressure are carried out to assembling block Power is added to 4-5GPa, and temperature is added to 1400-1600 DEG C, and pressure and temperature is kept for 24-72 hours, discharges pressure to 1 after stopping heat A atmospheric pressure takes out assembling block and is crushed, the metal blocks containing flaky graphite are taken out;
(5) flaky graphite is separated with metal progress pickling and extremely there is no bubble productions for heating distillation at 90-110 DEG C It is raw, high-graphitized carbon body is obtained by filtration;
(6) pickling is carried out after crushing high-graphitized carbon body again to bubble is no longer generated, is used repeatedly after filtering Clear water cleaning, finally obtains graphitized carbon powder;
(7) graphitized carbon powder is cleaned by ultrasonic, is dried to get the flaky graphite carbon body;
Above-mentioned metallic catalyst is the blocky simple substance of transition metal.
When using metallic catalyst catalysis biological carbon or graphitized carbon in the past, usually used catalyst is iron suicide, gold Belong to titanium, the dusty materials such as aluminium, usually by metal powder and biomass carbon or is difficult to graphitized carbon ferritic and mixes, then High temperature graphitization catalysis is carried out, is the high temperature graphitization catalysis carried out in no pressure or lower pressure condition, obtained graphite The degree of graphitization for changing carbon body is relatively low, and the carbon body obtained is spherical powder, and the present invention is with transition metal simple substance Catalyst extracts flaky graphite carbon body method in human hair and fills during extracting graphitized carbon from human hair Divide and consider problem of environmental pollution, do not use strong acid, strong base solution, does not use reducibility gas, oxidizing gas, be used only A certain amount of dilute nitric acid solution, greatly reduces the pollution to environment, in high temperature and pressure catalysis, uses transition metal catalyst To be catalyzed medium, so that catalytic condition is greatly lowered, compared under no catalysts conditions, graphitization temperature reduces 1000 DEG C, Transition metal-catalyzed medium has selected block materials rather than powder body material, under the extreme pressure that pressure reaches 4-5GPa, by it It is heated to melting temperature or more, reaches molten condition, biological carbon experienced after adequately dissolution precipitation process again, precipitation process sheet Carbon atom is realized in matter and completes the process rearranged, and the carbon of precipitation has physical chemistry identical with natural flake graphite Property.
Further, in step (1) roasting process exhaust emissions into sink.
It is that tail gas is discharged after water filters using above-mentioned further beneficial effect, prevents the gas of discharge to environment Pollution.
Further, solvent described in step (3) is the one or more for being saturated phenolic resin alcoholic solution, acetone soln, Additional amount is 4-10 times of biological carbon body quality.
It is using above-mentioned further beneficial effect, to be saturated phenolic resin alcoholic solution, acetone soln as solvent Facilitate powder granule molding.
Further, transition metal is fe, simple substance cobalt, elemental nickel or simple substance manganese, additional amount 10-50g, it is preferred that Metallic catalyst selects simple substance cobalt and elemental nickel, additional amount 10-50g.
It is using above-mentioned further beneficial effect, selects the catalytic activity of simple substance cobalt and elemental nickel high, so that catalysis Condition is greatly lowered, compared under no catalysts conditions, graphitization temperature reduces 1000 DEG C and the carbon that is precipitated have with The identical physicochemical properties of natural flake graphite, later period separating catalyst and graphitized carbon ferritic are also very easy, it is only necessary to Dust technology impregnates, and does not need electric furnace heating, and energy consumption is minimum.
Further, the condition of catalysis carbon deposition is in 1400-1600 DEG C of temperature and pressure 4.0-5.0GPa in step (4) Under, according to catalysis hair number, the time of catalysis is set, usually in 24-72h.
It is using above-mentioned further beneficial effect, concentration gradient diffusion principle is utilized under high-temperature and high-pressure conditions, it will Biomass carbon ferritic is placed in assembling block temperature end, and metallic catalyst is placed in low-temperature end, dissolves carbon in the catalyst dense It spends under the driving of gradient and diffuses to low-temperature end from temperature end, and crystallize precipitation in the form of graphite state in low-temperature end, to complete carbon Transformation of the element from unformed shape to crystalline state does not need to obtain flaky graphite using strong acid, strong base solution and reduction Property gas, oxidizing gas, greatly reduce the pollution to environment.
Further, assembling block includes transmission medium pyrophillite, dolomite insulating ring, sodium chloride ring, graphite heating pipe, oxidation Aluminium plug, magnesia blocking ring, conductive electrode and zirconium oxide blocking ring,
Two sides are equipped with opening through transmission medium pyrophillite formation cavity to transmission medium pyrophillite up and down, and transmission medium leaf is cured The opening at stone both ends seals to form reaction chamber with conductive electrode, is equipped with graphite heating pipe in reaction chamber, above and below graphite heating pipe Both ends are abutted with conductive electrode, cavity are equipped in graphite heating pipe, in cavity after the roasting again with aluminium oxide plug cladding Biological carbon dust and metallic catalyst, again roast after biological carbon dust be located at metallic catalyst top and be in close contact; It is successively arranged dolomite insulating ring, sodium chloride ring and zirconium oxide blocking ring between transmission medium pyrophillite and graphite heating pipe, reacts The vacant place in room is filled with the magnesia blocking ring of fixed graphite heating tube.
Above-mentioned structure be different from high-temperature and high-pressure conditions under temperature gradient method cultivate diamond used in assembling, related group Filling has biggish temperature gradient inside block, temperature gradient is set as 5-8 DEG C/mm, crystallization of the carbon body in metallic catalyst Rate control is in 30-80mg/h.Furthermore the design of the assembling can be stablized and be kept for 72 hours under 1600 DEG C of hot conditions.
Further, pickling is that pickling is carried out with the nitric acid solution of 20-37%, preferably carries out acid with 37% nitric acid solution It washes.
It is using above-mentioned further beneficial effect, carrying out pickling with the dust technology of 20-37% can effectively remove Metallic catalyst and other impurity.
Further, the operation being cleaned by ultrasonic in step (7) are as follows: graphitized carbon powder is immersed in dehydrated alcohol, with 30- The frequency of 40kHz carries out ultrasonic cleaning 10-30min.
It is using above-mentioned further beneficial effect, can effectively removes remaining acid solution, can guarantee graphitized carbon The purity of ferritic.
Detailed description of the invention
Fig. 1 is present invention assembling block structure sectional view;
Fig. 2 is the XRD diffracting spectrum of flaky graphite carbon body prepared by the embodiment of the present invention 1;
Fig. 3 is the XRD diffracting spectrum of flaky graphite carbon body prepared by the embodiment of the present invention 2.
In attached drawing, parts list represented by the reference numerals are as follows:
101, transmission medium pyrophillite;102, dolomite insulating ring;103, sodium chloride ring;104, graphite heating pipe;105, Aluminium oxide plug;106, magnesia blocking ring;107, conductive electrode;108, zirconium oxide blocking ring.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
In the examples below, structure chart such as Fig. 1 of block is assembled, assembling block includes transmission medium pyrophillite 101, dolomite Insulating ring 102, sodium chloride ring 103, graphite heating pipe 104, aluminium oxide plug 105, magnesia blocking ring 106,107 and of conductive electrode Zirconium oxide blocking ring 108,
About 101 two sides of transmission medium pyrophillite are equipped with opening and form cavity through transmission medium pyrophillite 101, and pressure transmission is situated between The opening at 101 both ends of matter pyrophillite forms reaction chamber with the sealing of conductive electrode 107, is equipped with graphite heating pipe 104 in reaction chamber, 104 upper and lower ends of graphite heating pipe are abutted with conductive electrode 107, and cavity is equipped in graphite heating pipe 104, has oxidation in cavity Biological carbon dust and metallic catalyst after the roasting again that aluminium plug 105 coats, the biological carbon dust after roasting again are located at Above metallic catalyst and it is in close contact;Dolomite guarantor is successively arranged between transmission medium pyrophillite 101 and graphite heating pipe 104 Warm ring 102, sodium chloride ring 103 and zirconium oxide blocking ring 108, the vacant place of reaction chamber are filled with the oxidation of fixed graphite heating tube 104 Magnesium blocking ring 106.
Other do not make the instrument of specified otherwise or reagent is the conventional instrument or reagent that existing channel can obtain.
Embodiment 1
(1) after taking human hair 20g to clean, 120 DEG C of holding 1h in drying box is put in and are then placed in oxidation to dry moisture In aluminium crucible, it is placed in atmosphere sintering furnace and is roasted and be continuously fed to fresh air, 370 DEG C of the temperature of roasting, heating rate 6 DEG C/min, calcining time 2h, obtain the first burning product of Organic biological carbon;
(2) the first burning product for obtaining Organic biological carbon are burnt boat with aluminium oxide ceramics to hold, is placed in vacuum tube furnace It being roasted, the condition of roasting is negative pressure 0.08MPa, and temperature is 1400 DEG C, heating rate 5.5 DEG C/min, calcining time 2h, Obtain biomass carbon ferritic;
(3) biomass carbon ferritic is subjected to ball milling with planetary ball mill, ball-milling medium is tungsten-carbide ball, and ball grinder is stainless The acetone soln dissolved with phenolic resin is then added in steel material, ball milling condition 1000r/min, time 1h, and additional amount is biology 4 times of carbon weight, phenolic resin content accounts for the 20% of biological carbon quality, after being sufficiently stirred, is placed on heating furnace and is dried Then dry-cure, drying time 1h obtain biological carbon dust to biological carbon ball milling again;
(4) it by biological carbon dust briquet shape, is roasted again in high-temperature tubular vacuum drying oven, roasting condition is negative pressure 0.08MPa, keeps the temperature 3h, the cylindric carbon body obtained after roasting by 900 DEG C of temperature, 5.5 DEG C/min of heating rate;
Carbon body is placed in assembling block, assembles the assembling mode of block as shown in Figure 1, assembling block size is 42*42* 42mm3, block internal cavity diameter 17mm is assembled, cylindrical iron block is placed in carbon body lower end, and iron block quality is 10g, for being catalyzed Assembling block is put in 420 cubic pressure machine equipment of φ and is heated, pressurizeed by graphitization, and temperature rises to 1500 DEG C, and pressure rises to 4GPa stops heat after keeping 36h, pressure is discharged to a standard atmospheric pressure, by broken metal of the taking-up containing graphite of assembling block Block.
(5) pickling separation is carried out with 37% nitric acid solution to flaky graphite and metallic iron, distillation is heated at 90 DEG C To there is no bubble generations, filters out acid solution and obtain high-graphitized carbon body;
(6) pickling is carried out to no longer generation gas with 37% nitric acid solution again after crushing high-graphitized carbon body Bubble after being filtered, is added clear water and rinses 3 times, finally obtain graphitized carbon powder;
(7) ultrasonic cleaning 30 minutes is carried out with the frequency of 30kHz to graphitized carbon powder, it is small is placed in 120 DEG C of drying boxes 1 Shi Jinhang is dried to get the flaky graphite carbon body, quality about 1.5g, XRD diffracting spectrum such as Fig. 2, the diffracting spectrum With a full set of graphite diffraction maximum, has no the diffraction maximum of other impurity elements, illustrate that the purity of carbon is very high.
Embodiment 2
(1) after taking human hair 50g to clean, 120 DEG C of holding 1h in drying box is put in and are then placed in oxidation to dry moisture It in aluminium crucible, is placed in atmosphere sintering furnace and is roasted and be continuously fed to fresh air, the temperature of roasting is 350 DEG C, heating speed Rate 6 DEG C/min, calcining time 3h obtain the first burning product of Organic biological carbon;
(2) the first burning product for obtaining Organic biological carbon are held with aluminium oxide ceramics container, is placed in vacuum tube furnace It being roasted, the condition of roasting is negative pressure 0.1MPa, and temperature is 1300 DEG C, heating rate 5.5 DEG C/min, calcining time 5h, Obtain biomass carbon ferritic;
(3) biomass carbon ferritic is subjected to ball milling with planetary ball mill, ball-milling medium is zirconia ball, and ball grinder is agate The absolute alcohol solution dissolved with phenolic resin is then added in material, ball milling condition 800r/min, time 2h, and additional amount is made a living 6 times of object carbon weight, the content of phenolic resin accounts for the 20% of biological carbon content, is sufficiently stirred to be placed on heating furnace and carries out Drying and processing, drying time 1h, again ball mill grinding obtain biological carbon dust;
(4) it by biological carbon dust briquet shape, is roasted again in high-temperature tubular vacuum drying oven, roasting condition is negative pressure 0.08MPa, keeps the temperature 3h, obtains cylindric carbon body by 1000 DEG C of temperature, 5.5 DEG C/min of heating rate;
Carbon body is placed in assembling block, assembles the assembling mode of block as shown in Figure 1, assembling block size is 64*64* 64mm3, block internal cavity diameter 32mm is assembled, cylindrical nickel block is placed in carbon body lower end to be catalyzed, and the quality of nickel block is 30g is used for catalyzed graphitization, and assembling block is put in 650 cubic hinge press of φ, is heated, is pressurizeed to assembling block, temperature liter To 1400 DEG C, pressure rises to 4GPa, stops heat after keeping 72h, pressure is discharged to a standard atmospheric pressure, and assembling block is crushed and is taken Out containing the metal blocks of graphite.
(5) pickling separation is carried out with 20% nitric acid solution to flaky graphite and heats distillation at 100 DEG C to no longer There is bubble generation, filter out acid solution, is rinsed carbon body 5 times with clear water, filter out moisture and obtain high-graphitized carbon body;
(6) pickling is carried out to no longer generation gas with 37% nitric acid solution again after crushing high-graphitized carbon body Bubble after being filtered, rinses crystalline flake graphite with clear water, finally obtains flaky graphite carbon body;
(7) ultrasonic cleaning 30 minutes is carried out with the frequency of 30kHz to graphitized carbon powder, dries 1 in 120 DEG C of drying boxes Hour to get the flaky graphite carbon body, quality is about 3.5g, XRD diffracting spectrum such as Fig. 3, which has A full set of graphite diffraction maximum, has no the diffraction maximum of other impurity elements, illustrates that the purity of carbon is very high.
Embodiment 3
(1) after taking human hair 100g to clean, 120 DEG C of holding 1h in drying box is put in and are then placed in oxygen to dry moisture Change in aluminium crucible, be placed in atmosphere sintering furnace and roasted and be continuously fed to fresh air, the temperature of roasting is 360 DEG C, heating Rate 5 DEG C/min, calcining time 3h obtain the first burning product of Organic biological carbon;
(2) the first burning product for obtaining Organic biological carbon are held with aluminium oxide ceramics container, is placed in vacuum tube furnace It is roasted, the condition of roasting is negative pressure 0.1MPa, and temperature is 1350 DEG C, heating rate 5 DEG C/min, and calcining time 5h is obtained To biomass carbon ferritic;
(3) biomass carbon ferritic is subjected to ball milling with planetary ball mill, ball-milling medium is zirconia ball, and ball grinder is agate The acetone soln dissolved with phenolic resin is then added in material, ball milling condition 1200r/min, time 0.5h, and additional amount is biology 10 times of carbon weight, the content of phenolic resin accounts for the 20% of biological carbon content, dries 1h using electric furnace after being sufficiently stirred, then Secondary ball mill grinding obtains biological carbon dust;
(4) it by biological carbon dust briquet shape, is roasted again in high-temperature tubular vacuum drying oven, roasting condition is negative pressure 0.1MPa, keeps the temperature 3h, obtains cylindric graphitized carbon ferritic by 900 DEG C of temperature, 5.5 DEG C/min of heating rate;
Carbon body is placed in assembling block, assembles the assembling mode of block as shown in Figure 1, assembling block size is 76*76* 76mm3, block internal cavity diameter 41mm is assembled, cylindrical cobalt block is placed in carbon body lower end, and quality 50g is used for catalytic graphite Change, it should be noted that when using pure cobalt as catalyst, alumina material 105 in assembling figure is needed replacing as magnesia Or zirconium oxide, reason are that pure cobalt can chemically react at high temperature with aluminium oxide.Assembling block is put in after being completed In 750 cubic hinge press of φ, assembling block is heated, is pressurizeed, temperature rises to 1400 DEG C, and pressure rises to 4GPa, after keeping 72h Stop heat, pressure is discharged to a standard atmospheric pressure, by broken metal blocks of the taking-up containing graphite of assembling block.
(5) flaky graphite and metallic cobalt are carried out pickling separation and heated at 100 DEG C to steam with 20% nitric acid solution Evaporate to there is no bubbles to generate, filter out acid solution, with clear water rinse carbon body 5 times, filter out moisture obtain it is high-graphitized Carbon body;
(6) pickling is carried out to no longer generation gas with 20% nitric acid solution again after crushing high-graphitized carbon body Bubble rinses crystalline flake graphite with clear water, finally obtains flaky graphite carbon body.
(7) ultrasonic cleaning 30min being carried out with the frequency of 40kHz to graphitized carbon powder, 120 DEG C of drying boxes are dried 1 hour, Up to the flaky graphite carbon body, quality is about 8g.

Claims (10)

1. a kind of extract flaky graphite carbon body method in human hair by catalyst of transition metal simple substance, feature exists In, comprising the following steps:
(1) it is put into alumina container after human hair being cleaned drying, is placed in atmosphere sintering furnace and roast and persistently send Enter fresh air, obtains the first burning product of Organic biological carbon;
(2) the first burning product for obtaining Organic biological carbon are held with aluminium oxide ceramics container, is placed in vacuum tube furnace and carries out Roasting, obtains biomass carbon ferritic;
(3) solvent will be added after biomass carbon ferritic ball milling, is dried after being sufficiently stirred, again ball mill grinding, obtains biological carbon dust End;
(4) by biological carbon dust briquet shape, metallic catalyst is added after roasting again in high-temperature tubular vacuum drying oven, is placed in Catalysis carbon deposition is carried out in assembling block, and heating pressurization is carried out to assembling block, utilizes transition metal-catalyzed biological carbon;
(5) pickling separation is carried out to flaky graphite and heats distillation to there is no bubble generation, be obtained by filtration high-graphitized Carbon body;
(6) will high-graphitized carbon body crush after carry out pickling again to bubble is no longer generated, filter out after acid solution repeatedly It is cleaned with clear water, finally filters out moisture content, obtain graphitized carbon ferritic;
(7) graphitized carbon powder is cleaned by ultrasonic, is dried to get the flaky graphite carbon body;
The metallic catalyst is the blocky simple substance of transition metal.
2. according to claim 1 a kind of using transition metal simple substance as flaky graphite in catalyst extraction human hair Carbon body method, which is characterized in that the temperature of roasting described in step (1) is 350-370 DEG C, 2-6 DEG C of heating rate/min, roasting The burning time is 2-5h.
3. according to claim 1 a kind of using transition metal simple substance as flaky graphite in catalyst extraction human hair Carbon body method, which is characterized in that the condition of roasting described in step (2) is negative pressure 0.08-0.1MPa, temperature 1300-1400 DEG C, 2-5.5 DEG C of heating rate/min, time 2-5h.
4. according to claim 1 a kind of using transition metal simple substance as flaky graphite in catalyst extraction human hair Carbon body method, which is characterized in that the operation of ball milling described in step (3) is to carry out ball milling with ball mill, and ball milling condition is 800-2000r/min, time 0.5-2h.
5. according to claim 1 a kind of using transition metal simple substance as flaky graphite in catalyst extraction human hair Carbon body method, which is characterized in that solvent described in step (3) is the one kind for being saturated phenolic resin alcoholic solution, acetone soln Or it is several, additional amount is 4-10 times of biomass carbonaceous amount.
6. according to claim 1 a kind of using transition metal simple substance as flaky graphite in catalyst extraction human hair Carbon body method, which is characterized in that roasting condition described in step (4) be negative pressure 0.08-0.1MPa, 900-1200 DEG C of temperature, 2-5.5 DEG C of heating rate/min keeps the temperature 2-5h;The transition metal is fe, simple substance cobalt, elemental nickel or simple substance manganese, is added Amount is 10-50g.
7. according to claim 1 a kind of using transition metal simple substance as flaky graphite in catalyst extraction human hair Carbon body method, which is characterized in that the condition that carbon deposition is catalyzed described in step (4) is 1400-1600 DEG C of temperature, pressure 4.0-5.0GPa sedimentation time 24-72h;
The assembling block includes that transmission medium pyrophillite (101), dolomite insulating ring (102), sodium chloride ring (103), graphite add Heat pipe (104), aluminium oxide plug (105), magnesia blocking ring (106), conductive electrode (107) and zirconium oxide blocking ring (108),
Two sides are equipped with opening through the transmission medium pyrophillite (101) formation chamber to the transmission medium pyrophillite (101) up and down The opening in road, transmission medium pyrophillite (101) both ends forms reaction chamber with the conductive electrode (107) sealing, described The graphite heating pipe (104), graphite heating pipe (104) upper and lower ends and the conductive electrode are equipped in reaction chamber (107) it abuts, cavity is equipped in the graphite heating pipe (104), there is the aluminium oxide plug (105) cladding in the cavity Again roast after biological carbon dust and metallic catalyst, again roast after biological carbon dust be located at metallic catalyst top And it is in close contact;The dolomite is successively arranged between the transmission medium pyrophillite (101) and the graphite heating pipe (104) Insulating ring (102), the sodium chloride ring (103) and the zirconium oxide blocking ring (108), the vacant place of reaction chamber is filled with fixation The magnesia blocking ring (106) of the graphite heating pipe (104).
8. according to claim 1 a kind of using transition metal simple substance as flaky graphite in catalyst extraction human hair Carbon body method, which is characterized in that pickling described in step (5) is to carry out pickling with the nitric acid solution of 20%-37%;It is described to add The temperature of thermal distillation is 90-110 DEG C.
9. according to claim 1 a kind of using transition metal simple substance as flaky graphite in catalyst extraction human hair Carbon body method, which is characterized in that pickling described in step (6) is to carry out pickling with the nitric acid solution of 20%-37%.
10. according to claim 1 a kind of using transition metal simple substance as flaky graphite in catalyst extraction human hair Change carbon body method, which is characterized in that the operation of ultrasonic cleaning described in step (7) are as follows: graphitized carbon powder is immersed in nothing In water-ethanol, ultrasonic cleaning 10-30min is carried out with the frequency of 30-40kHz.
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EP4206128A1 (en) * 2021-12-29 2023-07-05 Zhe Jiang Tip-Top Technology Co., Ltd. Method for extracting flake graphitized carbon body in human hair with transition metal alloy as catalyst
CN115253908A (en) * 2022-08-29 2022-11-01 洛阳美钻钻石培育有限公司 Method for artificially preparing biological diamond
CN115367731A (en) * 2022-08-29 2022-11-22 洛阳美钻钻石培育有限公司 Extraction process of biological carbon powder
CN115253908B (en) * 2022-08-29 2023-10-13 洛阳美钻新材料有限公司 Method for artificially preparing biological diamond
CN116425152A (en) * 2023-04-24 2023-07-14 昆明理工大学 Method for preparing high-purity graphite by iron adding refining
CN116425152B (en) * 2023-04-24 2024-05-10 昆明理工大学 Method for preparing high-purity graphite by iron adding refining

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