CN110156089A - A kind of preparation method of magnetic oxygenated graphene aerogel - Google Patents

A kind of preparation method of magnetic oxygenated graphene aerogel Download PDF

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Publication number
CN110156089A
CN110156089A CN201810114079.9A CN201810114079A CN110156089A CN 110156089 A CN110156089 A CN 110156089A CN 201810114079 A CN201810114079 A CN 201810114079A CN 110156089 A CN110156089 A CN 110156089A
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China
Prior art keywords
ferroso
graphene
ferric oxide
solution
magnetic oxygenated
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CN201810114079.9A
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车春玲
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Beijing Oumeizhong Science and Technology Research Institute
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Beijing Oumeizhong Science and Technology Research Institute
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Priority to CN201810114079.9A priority Critical patent/CN110156089A/en
Publication of CN110156089A publication Critical patent/CN110156089A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/08Ferroso-ferric oxide (Fe3O4)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/42Magnetic properties

Abstract

The invention belongs to technical field of function materials, and in particular to a kind of preparation method of magnetic oxygenated graphene aerogel.The preparation method of the magnetic oxygenated graphene aerogel, comprising the following steps: 1) graphene uniform ultrasonic disperse is subjected to oxidation processes in potassium persulfate solution, filtering drying is spare later, and graphene oxide is made;2) by ferroso-ferric oxide ultrasonic disperse in deionized water, ferroso-ferric oxide aqueous solution is made;3) ferroso-ferric oxide aqueous solution obtained in step 2 is mixed with the graphene oxide in step 1), and stirred evenly;4) ammonium hydroxide will be added in solution that step 3) stirs evenly to be stirred, magnetic oxygenated graphene aerogel is made.The beneficial effect is that: it is easy to operate, it is easy to accomplish industrialization has practical value outstanding, and bond strength is good, and stability is high, does not influence aeroge script quality, hopes the use demand for meeting all kinds of extreme environments.

Description

A kind of preparation method of magnetic oxygenated graphene aerogel
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of preparation side of magnetic oxygenated graphene aerogel Method.
Background technique
Magnetic porous material can be used for sewage treatment, target administration, microwave absorption (such as: radar absorbing material) field, Research significance is big, has received significant attention.Traditional absorbing material is mostly made of single ferrite, and ferrite is mostly with powder With coating material existing for the forms such as particle, although low in cost, simple process is difficult to meet light weight, absorption band wide Deng requiring, and because its density be easy to cause greatly under poor high temperature stability and hot environment and high band range in absorbing property difference etc. Disadvantage causes its application in the specific environments such as aircraft to be very restricted.Equally, in sewage treatment and target administration Equal fields, light porous magnetic material is more easily recycled, targeting easy to accomplish controls.Therefore, in order to meet multi-field answer This defect is overcome with demand, needs to prepare low-density, bigger serface, high intensity and magnetic material resistant to high temperature to meet Demand.
Summary of the invention
In order to compensate for the shortcomings of the prior art, the present invention provides a kind of preparation sides of magnetic oxygenated graphene aerogel Method.
The present invention is achieved through the following technical solutions:
A kind of preparation method of magnetic oxygenated graphene aerogel, comprising the following steps: 1) by graphene uniform ultrasonic disperse in Oxidation processes are carried out in potassium persulfate solution, filtering drying is spare later, be made graphene oxide, wherein potassium persulfate solution with The ratio of graphene is 1:2;
2) by ferroso-ferric oxide ultrasonic disperse in deionized water, the ratio of ferroso-ferric oxide and deionized water is 1:2, by super Sound dispersion is until be uniformly mixed, obtained ferroso-ferric oxide aqueous solution;
3) ferroso-ferric oxide aqueous solution obtained in step 2 is mixed with the graphene oxide in step 1), and stirred evenly;
4) ammonium hydroxide will be added in solution that step 3) stirs evenly to be stirred, the solution proportion that ammonium hydroxide and step 3) stir evenly It for 1:20, is then heat-treated in hydrothermal reaction kettle, heat treatment temperature is 80 DEG C~120 DEG C, and heat treatment time is 5~9 Hour, and dry cooling, magnetic oxygenated graphene aerogel is made.
The beneficial effects of the present invention are: a kind of preparation method of magnetic oxygenated graphene aerogel of the present invention is easy to operate, It being easily industrialized, there is practical value outstanding, and bond strength is good, stability is high, aeroge script quality is not influenced, Hope the use demand for meeting all kinds of extreme environments.
Specific embodiment
Specific embodiments of the present invention are given below, for further explaining the composition of the present invention.
Embodiment 1
A kind of preparation method of magnetic oxygenated graphene aerogel of the present invention, comprising the following steps: 1) by graphene uniform ultrasound It is scattered in potassium persulfate solution and carries out oxidation processes, filtering drying is spare later, graphene oxide is made, wherein potassium peroxydisulfate The ratio of solution and graphene is 1:2;
2) by ferroso-ferric oxide ultrasonic disperse in deionized water, the ratio of ferroso-ferric oxide and deionized water is 1:2, by super Sound dispersion is until be uniformly mixed, obtained ferroso-ferric oxide aqueous solution;
3) ferroso-ferric oxide aqueous solution obtained in step 2 is mixed with the graphene oxide in step 1), and stirred evenly;
4) ammonium hydroxide will be added in solution that step 3) stirs evenly to be stirred, the solution proportion that ammonium hydroxide and step 3) stir evenly It for 1:20, is then heat-treated in hydrothermal reaction kettle, heat treatment temperature is 80 DEG C, and heat treatment time is 5 hours, and dry It is cooling, magnetic oxygenated graphene aerogel is made.
Embodiment 2
A kind of preparation method of magnetic oxygenated graphene aerogel of the present invention, comprising the following steps: 1) by graphene uniform ultrasound It is scattered in potassium persulfate solution and carries out oxidation processes, filtering drying is spare later, graphene oxide is made, wherein potassium peroxydisulfate The ratio of solution and graphene is 1:2;
2) by ferroso-ferric oxide ultrasonic disperse in deionized water, the ratio of ferroso-ferric oxide and deionized water is 1:2, by super Sound dispersion is until be uniformly mixed, obtained ferroso-ferric oxide aqueous solution;
3) ferroso-ferric oxide aqueous solution obtained in step 2 is mixed with the graphene oxide in step 1), and stirred evenly;
4) ammonium hydroxide will be added in solution that step 3) stirs evenly to be stirred, the solution proportion that ammonium hydroxide and step 3) stir evenly It for 1:20, is then heat-treated in hydrothermal reaction kettle, heat treatment temperature is 100 DEG C, and heat treatment time is 7 hours, and is done Magnetic oxygenated graphene aerogel is made in dry cooling.
Embodiment 3
A kind of preparation method of magnetic oxygenated graphene aerogel of the present invention, comprising the following steps: 1) by graphene uniform ultrasound It is scattered in potassium persulfate solution and carries out oxidation processes, filtering drying is spare later, graphene oxide is made, wherein potassium peroxydisulfate The ratio of solution and graphene is 1:2;
2) by ferroso-ferric oxide ultrasonic disperse in deionized water, the ratio of ferroso-ferric oxide and deionized water is 1:2, by super Sound dispersion is until be uniformly mixed, obtained ferroso-ferric oxide aqueous solution;
3) ferroso-ferric oxide aqueous solution obtained in step 2 is mixed with the graphene oxide in step 1), and stirred evenly;
4) ammonium hydroxide will be added in solution that step 3) stirs evenly to be stirred, the solution proportion that ammonium hydroxide and step 3) stir evenly It for 1:20, is then heat-treated in hydrothermal reaction kettle, heat treatment temperature is 120 DEG C, and heat treatment time is 9 hours, and is done Magnetic oxygenated graphene aerogel is made in dry cooling.
The present invention is not limited to the above-described embodiments, anyone should learn make under the inspiration of the present invention with the present invention With same or similar technical solution, fall within the scope of protection of the present invention.
Technology not described in detail in the present invention, shape, construction portion are well-known technique.

Claims (2)

1. a kind of preparation method of magnetic oxygenated graphene aerogel, which comprises the following steps: 1) graphene is equal Even ultrasonic disperse carries out oxidation processes in potassium persulfate solution, and filtering drying is spare later, graphene oxide is made, wherein mistake The ratio of potassium sulfate solution and graphene is 1:2;
2) by ferroso-ferric oxide ultrasonic disperse in deionized water, the ratio of ferroso-ferric oxide and deionized water is 1:2, by super Sound dispersion is until be uniformly mixed, obtained ferroso-ferric oxide aqueous solution;
3) ferroso-ferric oxide aqueous solution obtained in step 2) is mixed with the graphene oxide in step 1), and stirred evenly;
4) ammonium hydroxide will be added in solution that step 3) stirs evenly to be stirred, the solution proportion that ammonium hydroxide and step 3) stir evenly It for 1:20, is then heat-treated in hydrothermal reaction kettle, heat treatment temperature is 80 DEG C~120 DEG C, and heat treatment time is 5~9 Hour, and dry cooling, magnetic oxygenated graphene aerogel is made.
2. the preparation method of a kind of magnetic oxygenated graphene aerogel according to claim 1, it is characterized in that: including following Step: 1) carrying out oxidation processes for graphene uniform ultrasonic disperse in potassium persulfate solution, and filtering drying is spare later, is made Graphene oxide, wherein the ratio of potassium persulfate solution and graphene is 1:2;
2) by ferroso-ferric oxide ultrasonic disperse in deionized water, the ratio of ferroso-ferric oxide and deionized water is 1:2, by super Sound dispersion is until be uniformly mixed, obtained ferroso-ferric oxide aqueous solution;
3) ferroso-ferric oxide aqueous solution obtained in step 2) is mixed with the graphene oxide in step 1), and stirred evenly;
4) ammonium hydroxide will be added in solution that step 3) stirs evenly to be stirred, the solution proportion that ammonium hydroxide and step 3) stir evenly It for 1:20, is then heat-treated in hydrothermal reaction kettle, heat treatment temperature is 100 DEG C, and heat treatment time is 7 hours, and is done Magnetic oxygenated graphene aerogel is made in dry cooling.
CN201810114079.9A 2018-02-05 2018-02-05 A kind of preparation method of magnetic oxygenated graphene aerogel Pending CN110156089A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111517774A (en) * 2020-04-28 2020-08-11 青岛迦南美地家居用品有限公司 Preparation method of magnetic graphene oxide aerogel
CN111569792A (en) * 2020-05-08 2020-08-25 中南大学 Aerogel composite material and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102185147A (en) * 2011-04-15 2011-09-14 南京师范大学 Nano iron phosphate hollow sphere/graphene composite material and preparation method thereof
CN103977748A (en) * 2014-05-23 2014-08-13 苏州大学 Magnetic aerogel and preparation method thereof
CN104258810A (en) * 2014-09-29 2015-01-07 扬州大学 Adsorbing agent based on ferroferric oxide and graphene and preparation method of adsorbing agent
CN105000886B (en) * 2015-07-13 2017-09-15 郑州大学 A kind of macroscopic three dimensional Fe3O4@graphene aerogels ultra light composite and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102185147A (en) * 2011-04-15 2011-09-14 南京师范大学 Nano iron phosphate hollow sphere/graphene composite material and preparation method thereof
CN103977748A (en) * 2014-05-23 2014-08-13 苏州大学 Magnetic aerogel and preparation method thereof
CN104258810A (en) * 2014-09-29 2015-01-07 扬州大学 Adsorbing agent based on ferroferric oxide and graphene and preparation method of adsorbing agent
CN105000886B (en) * 2015-07-13 2017-09-15 郑州大学 A kind of macroscopic three dimensional Fe3O4@graphene aerogels ultra light composite and preparation method

Non-Patent Citations (1)

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Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111517774A (en) * 2020-04-28 2020-08-11 青岛迦南美地家居用品有限公司 Preparation method of magnetic graphene oxide aerogel
CN111569792A (en) * 2020-05-08 2020-08-25 中南大学 Aerogel composite material and preparation method and application thereof

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Application publication date: 20190823