CN106732598A - The preparation method of carbon-encapsulated iron nanocatalyst - Google Patents
The preparation method of carbon-encapsulated iron nanocatalyst Download PDFInfo
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- CN106732598A CN106732598A CN201611043318.3A CN201611043318A CN106732598A CN 106732598 A CN106732598 A CN 106732598A CN 201611043318 A CN201611043318 A CN 201611043318A CN 106732598 A CN106732598 A CN 106732598A
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- China
- Prior art keywords
- carbon
- preparation
- sucrose
- hydrazine hydrate
- encapsulated iron
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000011943 nanocatalyst Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 23
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 35
- 229930006000 Sucrose Natural products 0.000 claims abstract description 35
- 239000005720 sucrose Substances 0.000 claims abstract description 35
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 31
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000243 solution Substances 0.000 claims abstract description 26
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000002604 ultrasonography Methods 0.000 claims abstract description 9
- 239000000919 ceramic Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000012467 final product Substances 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000003763 carbonization Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- 229940077388 benzenesulfonate Drugs 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 3
- -1 nitrates Sodium alkyl benzene Chemical class 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000005087 graphitization Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 5
- 238000005255 carburizing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002823 nitrates Chemical class 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 238000001241 arc-discharge method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- ZKEYULQFFYBZBG-UHFFFAOYSA-N lanthanum carbide Chemical compound [La].[C-]#[C] ZKEYULQFFYBZBG-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J33/00—Protection of catalysts, e.g. by coating
-
- B01J35/33—
-
- B01J35/40—
Abstract
The present invention relates to technical field of function materials, and in particular to a kind of preparation method of carbon-encapsulated iron nanocatalyst.The preparation method of carbon-encapsulated iron nanocatalyst, comprises the following steps:The first step, prepares the mixed solution and iron nitrate solution of sucrose and hydrazine hydrate;Second step, by iron nitrate solution with about 60 drops/point speed be added drop-wise in the mixed liquor of sucrose and hydrazine hydrate, while it is whole be added dropwise during sucrose and hydrazine hydrate mixed liquor keep ultrasound and stirring;3rd step, after after completion of dropping, the mixed solution of gained is placed in drying in baking oven and obtains presoma;4th step, be carbonized under presoma is loaded into ceramic crucible, nitrogen atmosphere, return goods after after cooling to room temperature, take out grinding obtain final product carbon-encapsulated iron nanocatalyst.Preferably, particle diameter distribution is 20 ~ 80 nm to carbon-encapsulated iron nanocatalyst dispersiveness of the present invention, and the average grain diameter of Fe nano-particles is 60 nm.Meanwhile, carbon thickness of the shell is about 5 nm, and degree of graphitization is relatively low, is amorphous state.
Description
Technical field
The present invention relates to technical field of function materials, and in particular to a kind of preparation method of carbon-encapsulated iron nanocatalyst.
Background technology
For catalyst field, reactivity high, target product selectivity high, mild reaction conditions, it is easily separated with
And the target for always being that it is pursued can be recycled.Respective masses are substantially better than experimental results demonstrate, nanocatalyst has
The catalysis activity of material, because nano material has, specific surface area is big, the undersaturated avtive spot of coordination of exposed surface
Many the features such as.Magnetic nano-catalyst has the characteristic of magnetic material, nano material and catalysis material concurrently, therefore always all
It is one of study hotspot of catalyst field.Carbon-clad metal nano particle is a kind of new carbon material, because of its unique core
Shell structure, can effectively prevent metal core oxidation in the environment, thus from 1993 by Ruoff arc discharge methods in sun
Since finding carbon coating lanthanum carbide in the cigarette ash of pole, one of study hotspot of carbon material always has been.Carbon-coated magnetic nanoparticle
The carbon shell that son has the advantage not available for independent magnetic nano-catalyst, i.e. nano grain surface cladding as catalyst can have
Effect prevents the catalyst from being influenceed by environment, effectively expands the magnetic catalyst scope of application.
The content of the invention
The present invention is directed to propose a kind of preparation method of carbon-encapsulated iron nanocatalyst.
Technical program of the present invention lies in:
The preparation method of carbon-encapsulated iron nanocatalyst, comprises the following steps:
The first step, prepares the mixed solution and iron nitrate solution of sucrose and hydrazine hydrate;
Second step, by iron nitrate solution with about 60 ~ 70 drops/point speed be added drop-wise in the mixed liquor of sucrose and hydrazine hydrate, while
Sucrose and hydrazine hydrate mixed liquor keep ultrasound and stirring during whole dropwise addition;
3rd step, after after completion of dropping, the mixed solution of gained is placed in drying in baking oven and obtains presoma;
4th step, be carbonized under presoma is loaded into ceramic crucible, nitrogen atmosphere, return goods after after cooling to room temperature, take out
Grinding obtains final product carbon-encapsulated iron nanocatalyst.
Described sucrose is with the preparation method of the mixed solution of hydrazine hydrate:The addition of sucrose is 6.0 ~ 30g, dodecane
The addition of base benzene sulfonic acid sodium salt is 0.3 ~ 0.5g, is subsequently adding distilled water and absolute ethyl alcohol, and fully dissolving obtains sucrose solution, so
It is added thereto to mass concentration again afterwards and is 70 ~ 80% ml of hydrazine hydrate solution 80, and adjusts the mixed solution of sucrose and hydrazine hydrate
PH value to 10, obtain the mixed liquor of sucrose and hydrazine hydrate.
Described regulation pH value is realized to when 10 by adding concentrated ammonia liquor.
Described distilled water and the volume ratio of absolute ethyl alcohol are 1:1.
The preparation method of described iron nitrate solution for add 6.059 ~ 6.063g ferric nitrates, be subsequently adding 50 ~ 80ml without
Water-ethanol, 0.3 ~ 0.5g neopelexes, ultrasound fully dissolving, obtain iron nitrate solution.
Described drying temperature is 80 DEG C.
Described carburizing temperature is 500 DEG C, the h of carbonization time 2.
Described annealing temperature is 1000 DEG C, the h of carbonization time 8.
The technical effects of the invention are that:
Preferably, particle diameter distribution is 20 ~ 80nm, the average grain diameter of Fe nano-particles to carbon-encapsulated iron nanocatalyst dispersiveness of the present invention
It is 60 nm.Meanwhile, carbon thickness of the shell is about 5 nm, and degree of graphitization is relatively low, is amorphous state.
Specific embodiment
The preparation method of carbon-encapsulated iron nanocatalyst, comprises the following steps:
Embodiment 1
The first step, prepares the mixed solution and iron nitrate solution of sucrose and hydrazine hydrate;
Second step, by iron nitrate solution with about 60 drops/point speed be added drop-wise in the mixed liquor of sucrose and hydrazine hydrate, while entirely
Sucrose and hydrazine hydrate mixed liquor keep ultrasound and stirring during dropwise addition;
3rd step, after after completion of dropping, the mixed solution of gained is placed in drying in baking oven and obtains presoma;
4th step, be carbonized under presoma is loaded into ceramic crucible, nitrogen atmosphere, return goods after after cooling to room temperature, take out
Grinding obtains final product carbon-encapsulated iron nanocatalyst.
Wherein, described sucrose is with the preparation method of the mixed solution of hydrazine hydrate:The addition of sucrose is 6.0g, 12
The addition of sodium alkyl benzene sulfonate is 0.3g, is subsequently adding distilled water and absolute ethyl alcohol, and fully dissolving obtains sucrose solution, then
The ml of hydrazine hydrate solution 80 that mass concentration is 70% is added thereto to again, and adjusts the pH value of sucrose and the mixed solution of hydrazine hydrate
To 10, the mixed liquor of sucrose and hydrazine hydrate is obtained.Described regulation pH value is realized to when 10 by adding concentrated ammonia liquor.Described steaming
The volume ratio of distilled water and absolute ethyl alcohol is 1:1.The preparation method of described iron nitrate solution is addition 6.059g ferric nitrates, then
50ml absolute ethyl alcohols, 0.3g neopelexes are added, ultrasound fully dissolving obtains iron nitrate solution.Described drying
Temperature is 80 DEG C.Described carburizing temperature is 500 DEG C, the h of carbonization time 2.Described annealing temperature is 1000 DEG C, carbonization time 8
h。
Embodiment 2
The first step, prepares the mixed solution and iron nitrate solution of sucrose and hydrazine hydrate;
Second step, by iron nitrate solution with about 60 drops/point speed be added drop-wise in the mixed liquor of sucrose and hydrazine hydrate, while entirely
Sucrose and hydrazine hydrate mixed liquor keep ultrasound and stirring during dropwise addition;
3rd step, after after completion of dropping, the mixed solution of gained is placed in drying in baking oven and obtains presoma;
4th step, be carbonized under presoma is loaded into ceramic crucible, nitrogen atmosphere, return goods after after cooling to room temperature, take out
Grinding obtains final product carbon-encapsulated iron nanocatalyst.
Wherein, described sucrose is with the preparation method of the mixed solution of hydrazine hydrate:The addition of sucrose is 30g, 12
The addition of sodium alkyl benzene sulfonate is 0.5g, is subsequently adding distilled water and absolute ethyl alcohol, and fully dissolving obtains sucrose solution, then
The ml of hydrazine hydrate solution 80 that mass concentration is 80% is added thereto to again, and adjusts the pH value of sucrose and the mixed solution of hydrazine hydrate
To 10, the mixed liquor of sucrose and hydrazine hydrate is obtained.Described regulation pH value is realized to when 10 by adding concentrated ammonia liquor.Described steaming
The volume ratio of distilled water and absolute ethyl alcohol is 1:1.The preparation method of described iron nitrate solution is addition 6.063g ferric nitrates, then
80ml absolute ethyl alcohols, 0.5g neopelexes are added, ultrasound fully dissolving obtains iron nitrate solution.Described drying
Temperature is 80 DEG C.Described carburizing temperature is 500 DEG C, the h of carbonization time 2.Described annealing temperature is 1000 DEG C, carbonization time 8
h。
Claims (8)
1. the preparation method of carbon-encapsulated iron nanocatalyst, it is characterised in that:Comprise the following steps:
The first step, prepares the mixed solution and iron nitrate solution of sucrose and hydrazine hydrate;
Second step, by iron nitrate solution with about 60 ~ 70 drops/point speed be added drop-wise in the mixed liquor of sucrose and hydrazine hydrate, while
Sucrose and hydrazine hydrate mixed liquor keep ultrasound and stirring during whole dropwise addition;
3rd step, after after completion of dropping, the mixed solution of gained is placed in drying in baking oven and obtains presoma;
4th step, be carbonized under presoma is loaded into ceramic crucible, nitrogen atmosphere, return goods after after cooling to room temperature, take out
Grinding obtains final product carbon-encapsulated iron nanocatalyst.
2. the preparation method of carbon-encapsulated iron nanocatalyst according to claim 1, it is characterised in that:Described sucrose with
The preparation method of the mixed solution of hydrazine hydrate is:The addition of sucrose is 6.0 ~ 30g, and the addition of neopelex is
0.3 ~ 0.5g, is subsequently adding distilled water and absolute ethyl alcohol, and fully dissolving obtains sucrose solution, quality is then added thereto to again dense
Spend the ml of hydrazine hydrate solution 80 for 70 ~ 80%, and adjust sucrose with the pH value of the mixed solution of hydrazine hydrate to 10, obtain sucrose with
The mixed liquor of hydrazine hydrate.
3. the preparation method of carbon-encapsulated iron nanocatalyst according to claim 1, it is characterised in that:Described regulation pH
Realized by adding concentrated ammonia liquor when being worth 10.
4. the preparation method of carbon-encapsulated iron nanocatalyst according to claim 2, it is characterised in that:Described distilled water
It is 1 with the volume ratio of absolute ethyl alcohol:1.
5. the preparation method of carbon-encapsulated iron nanocatalyst according to claim 1, it is characterised in that:Described ferric nitrate
The preparation method of solution is subsequently adding 50 ~ 80ml absolute ethyl alcohols, 0.3 ~ 0.5g 12 to add 6.059 ~ 6.063g ferric nitrates
Sodium alkyl benzene sulfonate, ultrasound fully dissolving, obtains iron nitrate solution.
6. the preparation method of carbon-encapsulated iron nanocatalyst according to claim 1, it is characterised in that:Described drying temperature
Spend is 80 DEG C.
7. the preparation method of carbon-encapsulated iron nanocatalyst according to claim 1, it is characterised in that:Described carbonization temperature
It is 500 DEG C to spend, the h of carbonization time 2.
8. the preparation method of carbon-encapsulated iron nanocatalyst according to claim 1, it is characterised in that:Described annealing temperature
It is 1000 DEG C to spend, the h of carbonization time 8.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108822919A (en) * | 2018-08-21 | 2018-11-16 | 方珺 | A kind of high-efficiency energy-saving nano boron liquid high perofmrnace lubricating oils and preparation method thereof |
CN109332681A (en) * | 2018-12-06 | 2019-02-15 | 河北工业大学 | Carbon-coated iron-tri-ferrous carbide magnetic nanoparticle preparation method |
-
2016
- 2016-11-24 CN CN201611043318.3A patent/CN106732598A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108822919A (en) * | 2018-08-21 | 2018-11-16 | 方珺 | A kind of high-efficiency energy-saving nano boron liquid high perofmrnace lubricating oils and preparation method thereof |
CN109332681A (en) * | 2018-12-06 | 2019-02-15 | 河北工业大学 | Carbon-coated iron-tri-ferrous carbide magnetic nanoparticle preparation method |
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WD01 | Invention patent application deemed withdrawn after publication |
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