CN106732598A - The preparation method of carbon-encapsulated iron nanocatalyst - Google Patents

The preparation method of carbon-encapsulated iron nanocatalyst Download PDF

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Publication number
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
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carbon
preparation
sucrose
hydrazine hydrate
encapsulated iron
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CN201611043318.3A
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Chinese (zh)
Inventor
李长英
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Shaanxi Jujiehan Chemical Co Ltd
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Shaanxi Jujiehan Chemical Co Ltd
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Priority to CN201611043318.3A priority Critical patent/CN106732598A/en
Publication of CN106732598A publication Critical patent/CN106732598A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74Iron group metals
    • B01J23/745Iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J33/00Protection 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

The preparation method of carbon-encapsulated iron nanocatalyst
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.
CN201611043318.3A 2016-11-24 2016-11-24 The preparation method of carbon-encapsulated iron nanocatalyst Pending CN106732598A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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

Cited By (2)

* Cited by examiner, † Cited by third party
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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