CN110482501A - A kind of method of reaction in-situ preparation carbon coating nitrided iron nano-powder - Google Patents
A kind of method of reaction in-situ preparation carbon coating nitrided iron nano-powder Download PDFInfo
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- CN110482501A CN110482501A CN201910867104.5A CN201910867104A CN110482501A CN 110482501 A CN110482501 A CN 110482501A CN 201910867104 A CN201910867104 A CN 201910867104A CN 110482501 A CN110482501 A CN 110482501A
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- ammonia
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0622—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with iron, cobalt or nickel
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The present invention relates to a kind of methods of reaction in-situ preparation carbon coating nitrided iron nano-powder, precursor solution A is prepared with molysite, water and dehydrated alcohol, it is dissolved in secondary distilled water with alkaline precipitating agent and prepares precursor solution B, the precipitating presoma obtained after precursor solution A and precursor solution B hybrid reaction is removed into Cl by deionized water filtration washing‑, use n-amyl alcohol to carry out azeotropic drying as azeotropic liquid, obtain the iron hydroxide dark red powder of n-amyl alcohol cladding；Then the iron hydroxide dark red powder that n-amyl alcohol coats is put into high pressure gas-solid reaction bed by carbonization and hydrogen reduction, nitrogen treatment, obtains carbon coating nitrided iron nano-powder.The present invention is easy to get with raw material, and preparation process is simple, efficient, safe, and energy saving, properties of product are stablized, the big advantage of batch output.
Description
Technical field
The present invention relates to technical field of preparation for inorganic material more particularly to a kind of reaction in-situ preparation carbon coating nitrided iron to receive
The method of rice flour body.
Background technique
Nitrided iron is because of specific capacity with higher and high charge-discharge efficiencies, good cyclical stability, after carbon coating
Can be applied to lithium ion battery negative material, also act as Hard Magnetic and soft magnetic material, information-recording material, magnetic seal liquid and
Catalysis material etc..Lithium ion battery has many advantages, such as that high voltage, small in size, light weight, energy density be big, good cycle, quilt
Being considered 21 century most has one of energy development project of application prospect.
Current lithium ion battery negative material is generally graphite alkenes material or using carbon as the material of matrix.Although carbon
Material has good performance in as lithium ion battery negative material, but its theoretical capacity is 372mAh/g, is limited
Its application in high-energy density demand electrochmical power source.Therefore, with the development of electronics industry and automotive field, merely
Theoretical capacity using carbon as cell negative electrode material can no longer meet the demand of every field, and possess higher specific volume
The nitrided iron of amount and high charge-discharge efficiencies, good cyclical stability just becomes new selection, combines following for carbon
The carbon coating nitrided iron nanocomposite of the height ratio capacity of ring stability and nitrided iron is conducive to negative in lithium ion battery
Application in the material of pole.
Patent disclosure (bulletin) number is that the Chinese patent of CN102623696A discloses a kind of " core-shell type carbon coating nitrided iron
Nano-complex particle preparation method and application " is evaporated block iron material using direct current arc hydrogen plasma equipment, is passed through simultaneously
A certain proportion of methane and argon gas obtain carbon-encapsulated iron nanoparticles presoma；The presoma is placed in 400 DEG C of ammonia atmosphere
Under carry out nitridation heat treatment 3~4h, obtain carbon coating nitrided iron nano-complex particle.The disadvantage is that: using direct-current arc hydrogen etc.
The method low output of block iron material, waste of energy, unfriendly to environment is evaporated in gas ions equipment.
Patent disclosure (bulletin) number is that the Chinese patent of CN103101892A discloses " a kind of carbon coating nitrogen without ammonia
Change the preparation method of iron nanometer powder ", nanometer iron powder is evenly dispersed in nitrogenous high polymeric solution, after washing solidification processing
Composite material precursor is obtained, after then the presoma is with or without oxidation processes, in high pure nitrogen or argon atmosphere
From room temperature with the heating rate continuous warming of 4~20 DEG C/min to 500~800 DEG C to get carbon coating nitrided iron nanometer powder.Its
The disadvantage is that used nanometer iron powder does not know how to obtain, and its reaction temperature is 500~800 DEG C, and such high temperature is difficult to prepare
Nanometer grade powder, and if argon gas meet high fever, container internal pressure increase, have the danger of cracking and explosion, industry metaplasia should not be carried out
It produces.
Summary of the invention
The present invention provides a kind of methods of reaction in-situ preparation carbon coating nitrided iron nano-powder, have raw material easy
, preparation process is simple, efficient, safe, and energy saving, properties of product are stablized, the big advantage of batch output.
In order to achieve the above object, the present invention is implemented with the following technical solutions:
A kind of method of reaction in-situ preparation carbon coating nitrided iron nano-powder, comprising the following steps:
1) the precursor preparation stage；
Prepared to obtain stable precursor solution A with molysite, water and dehydrated alcohol, specifically: after molysite is dissolved with water, first plus
Enter to account for the dehydrated alcohol of precursor solution A percent by volume 20%~40%, then solution be diluted to required concentration with deionized water,
Concentration range is 0.5~1.2mol/L；
It takes alkaline precipitating agent to be dissolved in and is configured to stable precursor solution B in secondary distilled water, the concentration of precursor solution B is
0.5~1.2mol/L；
By the precipitating presoma obtained after precursor solution A and precursor solution B hybrid reaction by deionized water filtration washing
Remove Cl-, use n-amyl alcohol to carry out azeotropic drying as azeotropic liquid, obtain the iron hydroxide dark red powder of n-amyl alcohol cladding；
2) carbonization and hydrogen reduction stage；
The iron hydroxide dark red powder that n-amyl alcohol coats is put into high pressure gas-solid reaction bed, first high pressure gas-solid reaction
High Purity Nitrogen gas is passed through 5~10 minutes in bed, displaces oxygen therein, then be passed through the mixed gas of ammonia and hydrogen, ammonia
Volume ratio with hydrogen is 1:2~3；The heating temperature for controlling high pressure gas-solid reaction bed is 250~350 DEG C, and pressure is maintained at 0.1
~0.8MPa, reaction time are 1~3h；
3) nitridation stage；
The heating temperature of high pressure gas-solid reaction bed is promoted to 350~450 DEG C, be passed through ammonia and hydrogen mixed gas or
The volume ratio of ammonia, ammonia and hydrogen is 3:1~0, and pressure is maintained at 0.1~0.8MPa, and the reaction time is 2~4h；Then lead to
Enter high pure nitrogen 5~10 minutes, closes drain tap, be cooled to room temperature in sealing；
Ethyl alcohol is passed through into the container equipped with reaction product to be passivated, it is final to obtain carbon coating nitrided iron nano powder
Body.
The molysite is FeCl3·6H2O、FeCl2·4H2O、Fe(NO3)3Or Fe2(SO4)3。
The alkaline precipitating agent is NaOH or NH3H2O。
The n-amyl alcohol is replaced with other alcohols materials not soluble in water, and other alcohols materials not soluble in water include positive fourth
Alcohol.
Compared with prior art, the beneficial effects of the present invention are:
It is easy to get with raw material, preparation process is simple, efficient, safe, and energy saving, properties of product are stablized, batch output
Big advantage.
Detailed description of the invention
Fig. 1 is the process schematic that the embodiment of the present invention 1 prepares carbon coating nitrided iron nano-powder.
Fig. 2 is the TEM figure of the cladding iron hydroxide of n-amyl alcohol described in the embodiment of the present invention 1.
Fig. 3 is carbon coating Fe prepared by the embodiment of the present invention 14The X ray diffracting spectrum of N nano-powder.
Fig. 4 is carbon coating Fe prepared by the embodiment of the present invention 23The X ray diffracting spectrum of N nano-powder.
Fig. 5 is carbon coating Fe prepared by the embodiment of the present invention 34N、Fe3The X ray diffracting spectrum of N nano-powder.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing:
A kind of method of reaction in-situ preparation carbon coating nitrided iron nano-powder of the present invention, comprising the following steps:
1) the precursor preparation stage；
Prepared to obtain stable precursor solution A with molysite, water and dehydrated alcohol, specifically: after molysite is dissolved with water, first plus
Enter to account for the dehydrated alcohol of precursor solution A percent by volume 20%~40%, then solution be diluted to required concentration with deionized water,
Concentration range is 0.5~1.2mol/L；
It takes alkaline precipitating agent to be dissolved in and is configured to stable precursor solution B in secondary distilled water, the concentration of precursor solution B is
0.5~1.2mol/L；
By the precipitating presoma obtained after precursor solution A and precursor solution B hybrid reaction by deionized water filtration washing
Remove Cl-, use n-amyl alcohol to carry out azeotropic drying as azeotropic liquid, obtain the iron hydroxide dark red powder of n-amyl alcohol cladding；
2) carbonization and hydrogen reduction stage；
The iron hydroxide dark red powder that n-amyl alcohol coats is put into high pressure gas-solid reaction bed, first high pressure gas-solid reaction
High Purity Nitrogen gas is passed through 5~10 minutes in bed, displaces oxygen therein, then be passed through the mixed gas of ammonia and hydrogen, ammonia
Volume ratio with hydrogen is 1:2~3；The heating temperature for controlling high pressure gas-solid reaction bed is 250~350 DEG C, and pressure is maintained at 0.1
~0.8MPa, reaction time are 1~3h；
3) nitridation stage；
The heating temperature of high pressure gas-solid reaction bed is promoted to 350~450 DEG C, be passed through ammonia and hydrogen mixed gas or
The volume ratio of ammonia, ammonia and hydrogen is 3:1~0, and pressure is maintained at 0.1~0.8MPa, and the reaction time is 2~4h；Then lead to
Enter high pure nitrogen 5~10 minutes, closes drain tap, be cooled to room temperature in sealing；
Ethyl alcohol is passed through into the container equipped with reaction product to be passivated, it is final to obtain carbon coating nitrided iron nano powder
Body.
The molysite is FeCl3·6H2O、FeCl2·4H2O、Fe(NO3)3Or Fe2(SO4)3。
The alkaline precipitating agent is NaOH or NH3H2O。
The n-amyl alcohol is replaced with other alcohols materials not soluble in water, and other alcohols materials not soluble in water include positive fourth
Alcohol.
Following embodiment is implemented under the premise of the technical scheme of the present invention, gives detailed embodiment and tool
The operating process of body, but protection scope of the present invention is not limited to following embodiments.Method therefor is such as without spy in following embodiments
Not mentionleting alone bright is conventional method.
[embodiment 1]
In the present embodiment, preparation carbon coating nitrided iron nano-powder specific steps are as follows:
1,1692 grams of FeCl are weighed3·6H2O is put into container, and it is molten to be configured to stable precursor with 8L water and 2L dehydrated alcohol
Liquid A；751.47 grams of sodium hydroxides are taken, is dissolved in 10L secondary distilled water and is configured to stable precursor solution B；By precursor solution
A, quick hybrid reaction obtains precipitating presoma to precursor solution B in the reactor, by deionized water filtration washing, using R system
Column Rotary Evaporators (industrial double conic rotary vacuum dryer) carry out azeotropic drying, and azeotropic liquid is n-amyl alcohol, azeotropic liquid dosage
1~1.5 times for precipitating presoma volume for solid obtains the iron hydroxide dark red powder (as shown in Figure 2) of n-amyl alcohol cladding.
2, as shown in Figure 1, the iron hydroxide dark red powder that n-amyl alcohol coats is put into high pressure gas-solid reaction bed, first
It is passed through nitrogen purge system 5 minutes, is then shut off nitrogen gas valve, then be passed through ammonia and hydrogen gas mixture (ammonia and hydrogen
The volume ratio of gas is 1:3), the heating temperature for controlling high pressure gas-solid reaction bed by heating power supply and thermocouple passes through at 350 DEG C
The flowmeter of exhaust end controls gas exit velocity, as pressure declines, then the mixed gas of ammonia and hydrogen is supplemented into system
(volume ratio of ammonia and hydrogen is 1:3, and mixed gas is mixed by High Purity Hydrogen and liquefied ammonia scene), system pressure is maintained at
0.3-0.4MPa determines the reaction time according to the inventory in reactor；The reaction time of the present embodiment is 1h, then in pressure
It is nitrogenized in the case where constant；
3, high pressure gas-solid reaction bed heating temperature is promoted to 400 DEG C, is passed through ammonia and hydrogen gas mixture (ammonia and hydrogen
The volume ratio of gas is 3:1), adjustment system pressure keeps system pressure constant in 0.3-0.4MPa, and temperature 2h is kept to be nitrogenized
Reaction, is passed through high pure nitrogen 5 minutes later.Drain tap is closed, is cooled to room temperature in sealing, reaction product is unloaded
Enter into storage tank, is then passed through ethyl alcohol into storage tank and is passivated, it is final to obtain carbon coating Fe4N nano-powder.
Carbon coating Fe prepared by the present embodiment4N nano-powder X ray diffracting spectrum is as shown in Figure 3.
[embodiment 2]
In the present embodiment, preparation carbon coating nitrided iron nano-powder specific steps are as follows:
Step 1, step 2 are the same as embodiment 1.
High pressure gas-solid reaction bed heating temperature is promoted to 400 DEG C by step 3, is passed through ammonia and hydrogen gas mixture (ammonia
Volume ratio with hydrogen is 3:0.8), pressure is adjusted within the scope of 0.3-0.4MPa, keeps system pressure constant, keeps temperature 2h
Nitridation reaction is carried out, is passed through high pure nitrogen later 5 minutes.Drain tap is closed, is cooled to room temperature in sealing, reaction
Object product is discharged into storage tank, is then passed through ethyl alcohol into storage tank and is passivated, final to obtain carbon coating Fe3N nanometers
Powder.
Carbon coating Fe prepared by the present embodiment4N nano-powder X ray diffracting spectrum is as shown in Figure 4.
[embodiment 3]
In the present embodiment, preparation carbon coating nitrided iron nano-powder specific steps are as follows:
Step 1, step 2 are the same as embodiment 1.
Step 3, high pressure gas-solid reaction bed heating temperature is promoted to 400 DEG C, is passed through ammonia and hydrogen gas mixture (ammonia
Volume ratio with hydrogen is 3:0.6), pressure is adjusted within the scope of 0.3-0.4MPa, keeps system pressure constant, keeps temperature 2h
Nitridation reaction is carried out, is passed through high pure nitrogen later 5 minutes.Drain tap is closed, is cooled to room temperature in sealing, reaction
Object product is discharged into storage tank, and ethyl alcohol is then passed through into storage tank for being passivated, finally obtains carbon coating Fe4N、Fe3N
The different nano-powder of content.
Carbon coating Fe prepared by the present embodiment4N、Fe3The different X ray diffracting spectrum of N content is as shown in Figure 5.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (4)
1. a kind of method of reaction in-situ preparation carbon coating nitrided iron nano-powder, which comprises the following steps:
1) the precursor preparation stage；
It is prepared to obtain stable precursor solution A with molysite, water and dehydrated alcohol, specifically: after molysite is dissolved with water, being first added and account for
The dehydrated alcohol of precursor solution A percent by volume 20%~40%, then solution is diluted to required concentration, concentration with deionized water
Range is 0.5~1.2mol/L；
It takes alkaline precipitating agent to be dissolved in and is configured to stable precursor solution B in secondary distilled water, the concentration of precursor solution B is 0.5
~1.2mol/L；
The precipitating presoma obtained after precursor solution A and precursor solution B hybrid reaction is removed by deionized water filtration washing
Cl-, use n-amyl alcohol to carry out azeotropic drying as azeotropic liquid, obtain the iron hydroxide dark red powder of n-amyl alcohol cladding；
2) carbonization and hydrogen reduction stage；
The iron hydroxide dark red powder that n-amyl alcohol coats is put into high pressure gas-solid reaction bed, first in high pressure gas-solid reaction bed
It is passed through High Purity Nitrogen gas 5~10 minutes, displaces oxygen therein, then be passed through the mixed gas of ammonia and hydrogen, ammonia and hydrogen
The volume ratio of gas is 1:2~3；The heating temperature for controlling high pressure gas-solid reaction bed is 250~350 DEG C, pressure is maintained at 0.1~
0.8MPa, reaction time are 1~3h；
3) nitridation stage；
The heating temperature of high pressure gas-solid reaction bed is promoted to 350~450 DEG C, is passed through the mixed gas or ammonia of ammonia and hydrogen
The volume ratio of gas, ammonia and hydrogen is 3:1~0, and pressure is maintained at 0.1~0.8MPa, and the reaction time is 2~4h；It then passes to
High pure nitrogen 5~10 minutes, drain tap is closed, is cooled to room temperature in sealing；
Ethyl alcohol is passed through into the container equipped with reaction product to be passivated, it is final to obtain carbon coating nitrided iron nano-powder.
2. a kind of method of reaction in-situ preparation carbon coating nitrided iron nano-powder according to claim 1, feature exist
In the molysite is FeCl3·6H2O、FeCl2·4H2O、Fe(NO3)3Or Fe2(SO4)3。
3. a kind of method of reaction in-situ preparation carbon coating nitrided iron nano-powder according to claim 1, feature exist
In the alkaline precipitating agent is NaOH or NH3H2O。
4. a kind of method of reaction in-situ preparation carbon coating nitrided iron nano-powder according to claim 1, feature exist
In the n-amyl alcohol is replaced with other alcohols materials not soluble in water, and other alcohols materials not soluble in water include n-butanol.
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| CN103101892A (en) * | 2013-03-08 | 2013-05-15 | 山东大学 | Preparation method of ammonia-gas-free carbon-coated iron nitride nanopowder |
| CN103145106A (en) * | 2013-01-29 | 2013-06-12 | 辽宁科技大学 | Preparation method of nitrided iron nano-powder and high-pressure gas-solid reaction bed thereof |
| CN103771512A (en) * | 2014-01-14 | 2014-05-07 | 辽宁科技大学 | Preparation method of metallic oxide nanometer powder |
| CN103794806A (en) * | 2014-01-27 | 2014-05-14 | 中南大学 | Nano iron nitride-carbon composite catalyst for positive electrode of lithium-air battery and preparation method of composite catalyst |
| CN106710762A (en) * | 2017-01-24 | 2017-05-24 | 北京工业大学 | Method for using nanometer iron nitride composite material in DNA (deoxyribonucleic acid) extraction |
-
2019
- 2019-09-12 CN CN201910867104.5A patent/CN110482501A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090324825A1 (en) * | 2008-05-30 | 2009-12-31 | Evenson Carl R | Method for Depositing an Aluminum Nitride Coating onto Solid Substrates |
| CN103145106A (en) * | 2013-01-29 | 2013-06-12 | 辽宁科技大学 | Preparation method of nitrided iron nano-powder and high-pressure gas-solid reaction bed thereof |
| CN103101892A (en) * | 2013-03-08 | 2013-05-15 | 山东大学 | Preparation method of ammonia-gas-free carbon-coated iron nitride nanopowder |
| CN103771512A (en) * | 2014-01-14 | 2014-05-07 | 辽宁科技大学 | Preparation method of metallic oxide nanometer powder |
| CN103794806A (en) * | 2014-01-27 | 2014-05-14 | 中南大学 | Nano iron nitride-carbon composite catalyst for positive electrode of lithium-air battery and preparation method of composite catalyst |
| CN106710762A (en) * | 2017-01-24 | 2017-05-24 | 北京工业大学 | Method for using nanometer iron nitride composite material in DNA (deoxyribonucleic acid) extraction |
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