CN104646044A - G-C3N4/NiFe2O4 composite material, as well as preparation method and application thereof - Google Patents

G-C3N4/NiFe2O4 composite material, as well as preparation method and application thereof Download PDF

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CN104646044A
CN104646044A CN201510082490.9A CN201510082490A CN104646044A CN 104646044 A CN104646044 A CN 104646044A CN 201510082490 A CN201510082490 A CN 201510082490A CN 104646044 A CN104646044 A CN 104646044A
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composite
preparation
nife2o4
ultrasonic disperse
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谈玲华
徐建华
杭祖圣
寇波
黄玉安
郏永强
王善斌
周家民
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Nanjing Institute of Technology
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Nanjing Institute of Technology
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Abstract

The invention discloses a g-C3N4/NiFe2O4 composite material, as well as a preparation method and application thereof, and belongs to the field of material preparation and energetic materials. The composition material is prepared by compositing g-C3N4 and nano NiFe2O4 at mass ratio of 99:1 to 90:10. The preparation method comprises the following steps: putting the nano NiFe2O4 in an ethanol solution to perform ultrasonic dispersion, adding the g-C3N4, performing the ultrasonic dispersion, continuously stirring in an ultrasonic procedure, slowly grinding the materials in an agate mortar to be pasty, drying the pasty material in a vacuum drying oven, roasting the dried material in a tube furnace to obtain the g-C3N4/NiFe2O4 composite material. The prepared g-C3N4/NiFe2O4 composite material shows excellent catalytic effect to thermal decomposition of ammonium perchlorate, so that the application field of graphite-phase carbon nitride is widened; according to the preparation method, the resource of the raw material is wide, the preparation process is simple, the production time is short and the preparation efficiency is high.

Description

A kind of g-C 3n 4/ NiFe 2o 4composite and its preparation method and application
Technical field
The invention belongs to material preparation and energetic material field, be specifically related to a kind of g-C 3n 4/ NiFe 2o 4the preparation method of composite, and use it for catalytic decomposition ammonium perchlorate (AP).
Background technology
Ammonium perchlorate (AP) is the high energy component in hydroxy-teminal butadiene (HTPB) composite solidpropellant, it accounts for the ratio of 60% ~ 80% in propellant, the combustibility of its thermal decomposition characteristic and propellant is closely related, can be inferred the combustibility of propellant by Study of Catalyst to the catalytic action of AP thermal decomposition.Research shows, material with carbon element, metal oxide, compound are used as the catalyst of ammonium perchlorate, can reduce the decomposition temperature of ammonium perchlorate or improve decomposition rate.Such as, [the Gu Kezhuan such as Gu, Deng. explosive wastewater journal, 2006,29,48] mix method and acetone by dry pigmentation, water and mix the standby compound of ammonium perchlorate (AP) with CNT (CNTs) of legal system, research shows that CNT (CNTs) has catalytic action to the burning of ammonium perchlorate and thermal decomposition.Yuan etc. [Yuan Y, et al.Applied Surface Science, 2014,303,354] adopt hydro-thermal method to prepare Fe 2o 3/ graphene composite, is reduced to 367 DEG C by the decomposition temperature of ammonium perchlorate.
G-C 3n 4be minimum energy in carbonitride, the most stable allotrope, have class graphite laminate structure and larger specific area, wherein nitrogen-atoms and carbon atom all belong to sp2 hydridization, there is the electronics moved freely in a large number between layers; Meanwhile, g-C 3n 4have that wearability is strong, chemical stability good, density is low, electric conductivity is high, cheap, advantages of environment protection, be considered to a kind of good catalyst and catalyst carrier.Nickel ferrite based magnetic loaded (NiFe 2o 4) be typical composite metal oxide, composite oxides in conjunction with the character of Multimetal oxide, thus can show the better catalytic performance of more single metal oxide in some aspects.Old grade [Chen Lijuan, etc. Materials Science and Engineering journal, 2012,30,591] adopt hydro-thermal method to prepare the NiFe of pure phase 2o 4the decomposition of nano particle to ammonium perchlorate has very high catalytic activity, and the decomposition temperature of AP is reduced to 350.8 DEG C.Primary Study, g-C 3n 4good catalytic effect is shown to the thermal decomposition of AP.In order to improve g-C further 3n 4catalytic activity, preparing its composite catalyst becomes research emphasis.Such as, Cao etc. [Cao S, et al.Applied Catalysis B:Environmental, 2014,147,940] utilize solvent-thermal method by In 2o 3be assembled in g-C 3n 4surface, obtains In 2o 3/ g-C 3n 4composite.This composite is used for photolysis water hydrogen, with pure g-C 3n 4catalyst is compared, and this composite effectively promotes the transfer efficiency of electric charge, improves the charge carrier life-span of light-catalyzed reaction.Zhou etc. [Zhou X, et al.Materials Research Bulletin, 2013,48, the 1447] Fe that utilized hydro-thermal method to prepare 3o 4/ g-C 3n 4nanosphere, research shows that this composite not only has obvious catalytic action to the degraded of target contaminant methyl orange, and has good magnetic and reusability.Based on above analysis, prepare g-C 3n 4/ NiFe 2o 4composite, effectively can improve catalyst activity, and ammonium perchlorate (AP) is decomposed at lower temperatures.
Summary of the invention
For solving the deficiencies in the prior art, the object of the invention is to, a kind of g-C is provided 3n 4/ NiFe 2o 4composite and preparation method thereof, and use it for catalytic decomposition ammonium perchlorate (AP), be preparation g-C 3n 4/ NiFe 2o 4composite provides a kind of new method, provides a kind of catalyst for ammonium perchlorate (AP) decomposes.
Originally for achieving the above object, the present invention adopts following technical scheme:
G-C provided by the present invention 3n 4/ NiFe 2o 4composite is with graphite phase carbon nitride g-C 3n 4as prop carrier, nano-Ni/Fe 2o 4uniform particles deposition is dispersed in g-C 3n 4surface, and g-C 3n 4with nano-Ni/Fe 2o 4mass ratio be 99:1 ~ 90:10.
Present invention also offers a kind of g-C 3n 4/ NiFe 2o 4the preparation method of composite, comprises the following steps:
(1) melamine or urea are prepared graphite phase carbon nitride (g-C by roasting, cooling, grinding 3n 4);
(2) by nano-Ni/Fe 2o 4be placed in ethanolic solution ultrasonic disperse, ultrasonic disperse is even, constantly stirs in ultrasonic procedure;
(3) by g-C prepared by step (1) 3n 4join in step (2) gained dispersion liquid and continue ultrasonic disperse, ultrasonic disperse is even, constantly stirs in ultrasonic procedure;
(4) mixture of step (3) is ground to pasty state at agate mortar, dries in vacuum, after roasting, obtain g-C 3n 4/ NiFe 2o 4composite.
In described step (2), the ultrasonic disperse time is 10 ~ 30 min.
In described step (3), the ultrasonic disperse time is 10 ~ 60 min.
In described step (4), milling time is 30 ~ 90 min.
Dry in described step (4) and adopt baking oven, vacuum drying temperature is 40 ~ 70 DEG C, and drying time is 4 ~ 6 h.
In described step (4), roasting adopts tube furnace, and sintering temperature is 150 ~ 350 DEG C, and roasting time is 30 ~ 90 min.
Present invention also offers a kind of g-C 3n 4/ NiFe 2o 4the application of composite, described g-C 3n 4/ NiFe 2o 4composite is used for the thermal decomposition of catalysis ammonium perchlorate (AP).
The present invention compared with prior art, has following beneficial effect:
(1) the present invention prepares g-C 3n 4/ NiFe 2o 4composite is applied to the thermal decomposition of catalysis ammonium perchlorate (AP), has widened g-C 3n 4application, simultaneously also for the catalytic decomposition of ammonium perchlorate (AP) have found a kind of new material.
(2) g-C is adopted 3n 4for prop carrier, at its surface deposition NiFe 2o 4nano particle, reduces NiFe 2o 4reunion probability, provide larger specific area and more activated centre, effectively improve the activity of catalysis ammonium perchlorate (AP) thermal decomposition.
(3) this method raw material sources are extensive, and preparation technology is simple, and the production time is short, and preparation efficiency is high, are applicable to industrialization large-scale production, have very high application prospect and practical value.
Accompanying drawing explanation
Fig. 1 is g-C prepared by embodiment 1 3n 4with g-C prepared by embodiment 3 3n 4/ NiFe 2o 4the XRD curve of composite;
Fig. 2 is g-C prepared by embodiment 1 3n 4scanning electron microscope diagram;
Fig. 3 is g-C prepared by embodiment 2 3n 4/ NiFe 2o 4the FT-IR curve of composite;
Fig. 4 is g-C prepared by embodiment 4 3n 4/ NiFe 2o 4the field emission scanning electron microscope figure of composite;
Fig. 5 is the Performance for Decomposition of Ammonium Perchlorate curve of embodiment 5, embodiment 6 and embodiment 7;
Fig. 6 is a kind of g-C of the present invention 3n 4/ NiFe 2o 4preparation method's flow chart of composite.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
embodiment 1preparation g-C 3n 4
Take 5 g melamines and put into ceramic crucible (covering crucible cover), in Muffle furnace, be warmed up to 500 DEG C with 50 DEG C/min, be incubated roasting 1 h at this temperature, be then rapidly heated in 5min 520 DEG C, insulation roasting 1 h, yellow powder sample is ground to obtain in cooling.
By material prepared by the method for embodiment 1, after x-ray diffractometer scanning, seeing Fig. 1, is g-C 3n 4.
By material prepared by the method for embodiment 1, through sem observation, see Fig. 2, the material of preparation is the g-C with layer structure 3n 4.
embodiment 2preparation g-C 3n 4/ NiFe 2o 4composite
as shown in Figure 6, a kind of g-C 3n 4/ NiFe 2o 4the preparation method of composite, comprises the following steps:
(1) graphite phase carbon nitride (g-C is prepared according to the method for embodiment 1 3n 4);
(2) by 0.01 g nano-Ni/Fe 2o 4be placed in 20 ml ethanolic solution ultrasonic disperse 10 min, constantly stir in ultrasonic procedure;
(3) g-C prepared by 0.99 g step (1) is taken 3n 4join in step (2) gained dispersion liquid and continue ultrasonic disperse 10 min, constantly stir in ultrasonic procedure;
(4) mixture of step (3) is ground 30 min to pasty state at agate mortar, put into vacuum drying oven 40 DEG C and dry 6 h, in tube furnace, 200 DEG C of roasting 30 min obtain g-C 3n 4/ NiFe 2o 4composite.
By g-C prepared by embodiment 2 3n 4/ NiFe 2o 4composite Fourier transform infrared collection of illustrative plates, is shown in Fig. 3, as can be seen from the figure, and 1645cm -1, 1240cm -1, 1321cm -1, 1411cm -1, 1564cm -1, 807cm -1for g-C 3n 4characteristic infrared absorption peak; 621cm -1, 400cm -1for NiFe 2o 4characteristic infrared absorption peak, meanwhile, g-C 3n 4/ NiFe 2o 4infrared curve in obviously can see g-C 3n 4absworption peak, and NiFe 2o 4absworption peak more weak, this is due to NiFe 2o 4the infrared absorption peak of self is more weak, simultaneously g-C 3n 4/ NiFe 2o 4niFe in composite 2o 4content is only 1% to be caused.FT-IR shows the g-C prepared 3n 4and NiFe 2o 4successfully to be compounded in together.
embodiment 3preparation g-C 3n 4/ NiFe 2o 4composite
as shown in Figure 6, a kind of g-C 3n 4/ NiFe 2o 4the preparation method of composite, comprises the following steps:
(1) graphite phase carbon nitride (g-C is prepared according to the method for embodiment 1 3n 4);
(2) by 0.05 g nano-Ni/Fe 2o 4be placed in 20 ml ethanolic solution ultrasonic disperse 20 min, constantly stir in ultrasonic procedure;
(3) g-C prepared by 0.95 g step (1) is taken 3n 4join in step (2) gained dispersion liquid and continue ultrasonic disperse 30 min, constantly stir in ultrasonic procedure;
(4) mixture of step (3) is ground 60 min to pasty state at agate mortar, put into vacuum drying oven 50 DEG C and dry 4 h, in tube furnace, 300 DEG C of roasting 1 h obtain g-C 3n 4/ NiFe 2o 4composite.
By g-C prepared by embodiment 3 3n 4/ NiFe 2o 4composite, after x-ray diffractometer scanning, is shown in Fig. 1, from g-C 3n 4/ NiFe 2o 4g-C can be found in the XRD curve of composite 3n 4and NiFe 2o 4characteristic diffraction peak, this sign show prepare material be g-C 3n 4/ NiFe 2o 4composite.
embodiment 4preparation g-C 3n 4/ NiFe 2o 4composite
as shown in Figure 6, a kind of g-C 3n 4/ NiFe 2o 4the preparation method of composite, comprises the following steps:
(1) graphite phase carbon nitride (g-C is prepared according to the method for embodiment 1 3n 4);
(2) by 0.1 g nano-Ni/Fe 2o 4be placed in 20 ml ethanolic solution ultrasonic disperse 30 min, constantly stir in ultrasonic procedure;
(3) g-C prepared by 0.9 g step (1) is taken 3n 4join in step (2) gained dispersion liquid and continue ultrasonic disperse 60 min, constantly stir in ultrasonic procedure;
(4) mixture of step (3) is ground 90 min to pasty state at agate mortar, put into vacuum drying oven 60 DEG C and dry 6 h, in tube furnace, 350 DEG C of roasting 90 min obtain g-C 3n 4/ NiFe 2o 4composite.
By g-C prepared by embodiment 4 3n 4/ NiFe 2o 4composite, through after sem observation, is shown in Fig. 4, NiFe 2o 4be dispersed in g-C uniformly 3n 4surface, nano-Ni/Fe 2o 4there is a small amount of agglomeration.
embodiment 5g-C 3n 4/ NiFe 2o 4the application of composite catalysis ammonium perchlorate (AP) thermal decomposition
G-C prepared by Example 3 3n 4/ NiFe 2o 4composite 0.1g adds in ethanol and stirs together with 0.99 g ammonium perchlorate (AP), mixes, and after dry, sampling 9-10 mg tests TGA-DTA, test condition: argon gas atmosphere, flow: 20 ml/min, heating rate 10 DEG C/min, temperature range: 100-500 DEG C.Test result is shown in Fig. 5, and high-temperature decomposition temperature is 404.1 DEG C.
embodiment 6g-C 3n 4/ NiFe 2o 4the application of composite catalysis ammonium perchlorate (AP) thermal decomposition
G-C prepared by Example 3 3n 4/ NiFe 2o 4composite 0.3g adds in ethanol and stirs together with 0.97 g ammonium perchlorate (AP), mixes, and after dry, sampling 9-10 mg tests TGA-DTA, test condition: argon gas atmosphere, flow: 20 ml/min, heating rate 10 DEG C/min, temperature range: 100-500 DEG C.Test result is shown in Fig. 5, and high-temperature decomposition temperature is 388.5 DEG C.
embodiment 7g-C 3n 4/ NiFe 2o 4the application of composite catalysis ammonium perchlorate (AP) thermal decomposition
G-C prepared by Example 3 3n 4/ NiFe 2o 4composite 0.5 g adds in ethanol and stirs together with 0.95 g ammonium perchlorate (AP), mixes, and after dry, sampling 9-10 mg tests TGA-DTA, test condition: argon gas atmosphere, flow: 20 ml/min, heating rate 10 DEG C/min, temperature range: 100-500 DEG C.Test result is shown in Fig. 5, and high-temperature decomposition temperature is 382.1 DEG C.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and distortion, these improve and distortion also should be considered as protection scope of the present invention.

Claims (8)

1. a g-C 3n 4/ NiFe 2o 4composite, is characterized in that, with graphite phase carbon nitride g-C 3n 4as prop carrier, nano-Ni/Fe 2o 4uniform particles deposition is dispersed in g-C 3n 4surface, and g-C 3n 4with nano-Ni/Fe 2o 4mass ratio be 99:1 ~ 90:10.
2. a kind of g-C according to claim 1 3n 4/ NiFe 2o 4the preparation method of composite, is characterized in that, comprises the following steps:
(1) melamine or urea are prepared graphite phase carbon nitride g-C by roasting, cooling, grinding 3n 4;
(2) by nano-Ni/Fe 2o 4be placed in ethanolic solution ultrasonic disperse, ultrasonic disperse is even, constantly stirs in ultrasonic procedure;
(3) by g-C prepared by step (1) 3n 4join in step (2) gained dispersion liquid and continue ultrasonic disperse, ultrasonic disperse is even, constantly stirs in ultrasonic procedure;
(4) mixture of step (3) is ground to pasty state at agate mortar, dries in vacuum, after roasting, obtain g-C 3n 4/ NiFe 2o 4composite.
3. a kind of g-C according to claim 2 3n 4/ NiFe 2o 4the preparation method of composite, is characterized in that: in step (2), the ultrasonic disperse time is 10 ~ 30 min.
4. a kind of g-C according to claim 2 3n 4/ NiFe 2o 4the preparation method of composite, is characterized in that: in step (3), the ultrasonic disperse time is 10 ~ 60 min.
5. a kind of g-C according to claim 2 3n 4/ NiFe 2o 4the preparation method of composite, is characterized in that: in step (4), milling time is 30 ~ 90 min.
6. a kind of g-C according to claim 2 3n 4/ NiFe 2o 4the preparation method of composite, is characterized in that: dry in step (4) and adopt baking oven, vacuum drying temperature is 40 ~ 70 DEG C, and drying time is 4 ~ 6 h.
7. a kind of g-C according to claim 2 3n 4/ NiFe 2o 4the preparation method of composite, is characterized in that: in step (4), roasting adopts tube furnace, and sintering temperature is 150 ~ 350 DEG C, and roasting time is 30 ~ 90 min.
8. a kind of g-C according to claim 1 3n 4/ NiFe 2o 4the application of composite, is characterized in that, described g-C 3n 4/ NiFe 2o 4composite is used for the thermal decomposition of catalysis ammonium perchlorate.
CN201510082490.9A 2015-02-15 2015-02-15 G-C3N4/NiFe2O4 composite material, as well as preparation method and application thereof Pending CN104646044A (en)

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CN106378171A (en) * 2016-08-17 2017-02-08 浙江工业大学 A method of preparing a magnetic ZnFe<2>O4/g-C3N4 composite photocatalytic material
CN106563485A (en) * 2016-11-08 2017-04-19 江苏大学 Carbon nitride/potassium calcium niobate composite material and preparing method and application thereof
CN106861739A (en) * 2015-12-11 2017-06-20 中国科学院大连化学物理研究所 A kind of hollow core-shell type magnetic mesoporous carbonitride and preparation method thereof
CN109052344A (en) * 2018-07-24 2018-12-21 江苏理工学院 A kind of preparation method of graphite phase carbon nitride/nickel oxide composite material
CN110243880A (en) * 2019-07-11 2019-09-17 蚌埠学院 A kind of preparation method and application for the gas sensitive detecting ammonia
CN112174100A (en) * 2020-09-29 2021-01-05 桂林理工大学 Multilayer egg roll-like compound superhard facies C3N4Nanotube and method for preparing the same
CN114984258A (en) * 2021-03-02 2022-09-02 中国农业科学院油料作物研究所 Green method for efficiently inhibiting growth of aspergillus flavus spores producing toxin

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CN105289692A (en) * 2015-11-19 2016-02-03 南京工程学院 g-C3N4/Fe2O3 composite material and its preparation method and use
CN106861739A (en) * 2015-12-11 2017-06-20 中国科学院大连化学物理研究所 A kind of hollow core-shell type magnetic mesoporous carbonitride and preparation method thereof
CN106378171A (en) * 2016-08-17 2017-02-08 浙江工业大学 A method of preparing a magnetic ZnFe<2>O4/g-C3N4 composite photocatalytic material
CN106378171B (en) * 2016-08-17 2019-03-08 浙江工业大学 A kind of magnetism ZnFe2O4/g-C3N4The preparation method of composite photocatalyst material
CN106563485A (en) * 2016-11-08 2017-04-19 江苏大学 Carbon nitride/potassium calcium niobate composite material and preparing method and application thereof
CN109052344A (en) * 2018-07-24 2018-12-21 江苏理工学院 A kind of preparation method of graphite phase carbon nitride/nickel oxide composite material
CN110243880A (en) * 2019-07-11 2019-09-17 蚌埠学院 A kind of preparation method and application for the gas sensitive detecting ammonia
CN110243880B (en) * 2019-07-11 2021-10-12 蚌埠学院 Preparation method and application of gas-sensitive material for detecting ammonia gas
CN112174100A (en) * 2020-09-29 2021-01-05 桂林理工大学 Multilayer egg roll-like compound superhard facies C3N4Nanotube and method for preparing the same
CN114984258A (en) * 2021-03-02 2022-09-02 中国农业科学院油料作物研究所 Green method for efficiently inhibiting growth of aspergillus flavus spores producing toxin
CN114984258B (en) * 2021-03-02 2023-09-26 中国农业科学院油料作物研究所 Green method for efficiently inhibiting growth of toxic aspergillus flavus spores

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