CN104692344A - Preparation method of mesoporous graphite-phase carbon nitride material - Google Patents
Preparation method of mesoporous graphite-phase carbon nitride material Download PDFInfo
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- CN104692344A CN104692344A CN201510083075.5A CN201510083075A CN104692344A CN 104692344 A CN104692344 A CN 104692344A CN 201510083075 A CN201510083075 A CN 201510083075A CN 104692344 A CN104692344 A CN 104692344A
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- carbon nitride
- phase carbon
- nitride material
- mesoporous graphite
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Abstract
The invention discloses a preparation method of a mesoporous graphite-phase carbon nitride material. The material is prepared by using a monocyanamide water solution as a raw material and nano colloid SiO2 as a template by a hard template process. The preparation method comprises the following steps: adding nano colloid oxidized SiO2 into a monocyanamide water solution, stirring uniformly, drying and calcining to obtain light yellow powder; putting the powder into an NH4HF2 solution, and stirring to remove the SiO2 template; and washing, and drying to obtain the mesoporous graphite-phase carbon nitride (mpg-C3H4) material. Compared with the common blocky graphite-phase carbon nitride (g-C3H4) material, the mesoporous graphite-phase carbon nitride (mpg-C3H4) material has larger specific area, and thus, has better catalytic effect on thermal decomposition of ammonium perchlorate. The preparation method has the advantages of simple technical operation, wide raw material sources and high preparation efficiency.
Description
Technical field
The present invention relates to a kind of mesoporous graphite phase carbon nitride (mpg-C
3n
4) preparation method of material, belong to material preparation and energetic material field.
Background technology
Class graphitic carbon nitride (g-C
3n
4) because of its special physical and chemical performance, cause the extensive concern of researcher, have broad application prospects in fields such as photochemical catalysis, Solar use, environment protection, heterogeneous catalysts, be considered to the Multifunction material that can replace conventional carbon material.But, g-C
3n
4the pore structure of material and its performance of specific surface area extreme influence, in general, g-C
3n
4specific surface higher, the active site provided is more, and catalytic performance is better.Adopt g-C prepared by traditional method
3n
4mostly block in layer, specific surface area is less, lamellar spacing is comparatively large, thus limits g-C
3n
4application.By mesoporous graphite phase carbon nitride (mpg-C prepared by hard template method
3n
4) material, the meso-hole structure of the 2-50 nm be rich in material, has large specific surface area, meanwhile, and mpg-C
3n
4electronic Structure Characteristics can promote in catalytic reaction process transfer transport, promoter action is played to the mass transfer diffusion in reaction, thus shows better catalytic effect.
Ammoniumper chlorate (AP) is the high energy component in compositepropellent, it accounts for the ratio of about 60% in propelling agent, the combustionproperty of its thermal decomposition characteristic and propelling agent is closely related, can be inferred the combustionproperty of propelling agent by Study of Catalyst to the katalysis of AP thermolysis.Research shows, carbon material is to the good katalysis of the thermolysis of ammoniumper chlorate (AP).Such as, [Zhang W W, the et al.Materials Research Bulletin such as Zhang, 2014,50,73] adopt nitric-sulfuric acid to carry out nitratedly having prepared nitration oxidation Graphene (NGO) to graphene oxide, make the high-temperature decomposition temperature of ammoniumper chlorate be down to 326 DEG C; Cui etc. [Cui Ping, etc. explosive wastewater journal, 2006,29,25] prepare carbon nanotube (CNTs)/AP composite particles by solvent evaporated method, the high-temperature decomposition temperature of ammoniumper chlorate is reduced 113.9 DEG C.Based on above analysis, the mesoporous graphite phase carbon nitride (mpg-C that the present invention adopts hard template method to prepare
3n
4), there is better katalysis to the thermolysis of ammoniumper chlorate (AP).
Summary of the invention
For solving the deficiencies in the prior art, the object of the invention is to, a kind of preparation method of mesoporous graphite phase carbon nitride material is provided, for preparing the class graphite phase carbon nitride (g-C of specific morphology
3n
4) material provides a kind of new method; Mesoporous graphite phase carbon nitride (the mpg-C prepared in this way
3n
4) material and general block g-C
3n
4material is compared, mpg-C
3n
4material has larger specific surface area, thus shows better catalytic effect to the thermolysis of ammoniumper chlorate.
The invention provides a kind of preparation method of mesoporous graphite phase carbon nitride material, comprise the following steps:
(1) nanometer colloidal silica is put into the cyanamide aqueous solution, stirring at room temperature, make it mix fully;
(2) mixed solution of step (1) is left standstill, remove supernatant liquid and be placed on dry white solid in baking oven;
(3) by the white solid porphyrize that step (2) obtains, after being placed in retort furnace calcining, pale yellow powder is ground to obtain;
(4) pale yellow powder that step (3) obtains is scattered in NH
4hF
2stir in solution, deionized water and washing with alcohol, dry mpg-C
3n
4material.
In described step (1), the cyanamide aqueous solution is 5 ~ 15 g, and nanometer colloidal silica is 10 ~ 40 g.
In described step (1), churning time is 2 ~ 4 h.
In described step (2), drying temperature is 40 ~ 70 DEG C.
In described step (3), calcining temperature is 400 ~ 600 DEG C, and the time is 3 ~ 6 h.
NH in described step (4)
4hF
2the concentration of solution is 2 ~ 5 mol/L.
NH in described step (4)
4hF
2the consumption of solution is 100 ~ 400 mL.
In described step (4), churning time is 48 ~ 64 h.
In described step (4), washing times is 1 ~ 4 time.
In described step (4), drying temperature is 40 ~ 70 DEG C, and the time is 1 ~ 3 h.
The present invention compared with prior art, has following beneficial effect:
(1) mpg-C adopting present method to prepare
3n
4with general block g-C
3n
4compare, there is larger specific surface area, provide active site more, effectively improve the activity of catalysis ammoniumper chlorate (AP) thermolysis.
(2) mpg-C adopting present method to prepare
3n
4materials application, in the thermolysis of catalysis ammoniumper chlorate (AP), has widened g-C
3n
4application Areas, simultaneously also for the catalytic decomposition of ammoniumper chlorate (AP) have found a kind of efficient catalyst.
(3) present method raw material sources are extensive, and preparation technology is simple, are applicable to industrialization scale operation, have very high application prospect and practical value in energetic material field.
Accompanying drawing explanation
Fig. 1 is mpg-C prepared by embodiment 1
3n
4fT-IR curve.
Fig. 2 is mpg-C prepared by embodiment 2
3n
4xRD curve.
Fig. 3 is mpg-C prepared by embodiment 2
3n
4tEM picture.
Fig. 4 is block g-C
3n
4with mpg-C prepared by embodiment 2
3n
4the performance test curve of Catalytic Performance for Decomposition of Ammonium Perchlorate.
Fig. 5 is a kind of mpg-C of the present invention
3n
4preparation method's schema of material.
Embodiment
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 1
As shown in Figure 5, a kind of preparation method of mesoporous graphite phase carbon nitride material, comprises the following steps:
(1) 10 g nanometer colloidal state SiO are taken
2put into the cyanamide aqueous solution that 5 g concentration are 50 wt%, at room temperature stir 4 h and make it mix fully;
(2) mixed solution of step (1) is left standstill, remove supernatant liquid and to be placed in baking oven 60 DEG C of dry white solids;
(3) by the white solid porphyrize that step (2) obtains, after being placed in retort furnace 500 DEG C calcining 6 h, pale yellow powder is ground to obtain;
(4) pale yellow powder that step (3) obtains is scattered in the NH that 400 mL concentration are 2 mol/L
4hF
2stir 64 h in solution, deionized water and ethanol respectively wash 1 time, 70 DEG C drying 1 h and obtain mpg-C
3n
4material.
By mpg-C prepared by embodiment 1
3n
4material, observes through Fourier transform infrared collection of illustrative plates, sees Fig. 1, as can be seen from the figure, and 1240 cm
-1, 1321 cm
-1, 1411 cm
-1, 1564 cm
-1, 1645 cm
-1, 807 cm
-1for mpg-C
3n
4characteristic infrared absorption peak; FT-IR shows the mpg-C prepared
3n
4and g-C
3n
4the same, there is graphite-like structure.
embodiment 2
as shown in Figure 5, a kind of preparation method of mesoporous graphite phase carbon nitride material, comprises the following steps:
(1) 30 g nanometer colloidal state SiO are taken
2put into the cyanamide aqueous solution that 10 g concentration are 50 wt%, at room temperature stir 2 h and make it mix fully;
(2) mixed solution of step (1) is left standstill, remove supernatant liquid and to be placed in baking oven 50 DEG C of dry white solids;
(3) by the white solid porphyrize that step (2) obtains, after being placed in retort furnace 550 DEG C calcining 4 h, pale yellow powder is ground to obtain;
(4) pale yellow powder that step (3) obtains is scattered in the NH that 200 mL concentration are 4 mol/L
4hF
2stir 48 h in solution, deionized water and ethanol respectively wash 2 times, 50 DEG C drying 2 h and obtain mpg-C
3n
4material.
By material prepared by the method for embodiment 2, after x-ray diffractometer scanning, see Fig. 2, the mpg-C of preparation
3n
4and g-C
3n
4the same, there is graphite-like structure.
By mpg-C prepared by the method for embodiment 2
3n
4material, through transmission electron microscope observation, is shown in Fig. 3, and the material of preparation is the mpg-C simultaneously with laminate structure and vermiform pore structure
3n
4.
Prepared mpg-C
3n
4the performance test of material is as follows: mpg-C prepared by Example 2
3n
4material 0.2g adds in dehydrated alcohol and stirs together with 0.98 g ammoniumper chlorate (AP), mixes, and after dry, sampling 9-10 mg tests DTA, test condition: argon gas atmosphere, flow: 20 ml/min, temperature rise rate 10 DEG C/min, temperature range: 100-500 DEG C.Test result is shown in Fig. 4, and high-temperature decomposition temperature is 337.8 DEG C.Equally, g-C prepared by usual way is got
3n
4material 0.2g adds in dehydrated alcohol and stirs together with 0.98 g ammoniumper chlorate (AP), mixes, and after dry, sampling 9-10 mg tests DTA, test condition: argon gas atmosphere, flow: 20 ml/min, temperature rise rate 10 DEG C/min, temperature range: 100-500 DEG C.Test result is shown in Fig. 4, and high-temperature decomposition temperature is 394.2 DEG C.Mesoporous graphite phase carbon nitride (the mpg-C that a process for preparing is described
3n
4) with general block g-C
3n
4compare, to the catalytic decomposition of ammoniumper chlorate, there is better catalytic effect, AP is decomposed at lower temperatures.
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 (10)
1. a preparation method for mesoporous graphite phase carbon nitride material, is characterized in that, comprise the following steps:
(1) nanometer colloidal silica is put into the cyanamide aqueous solution, stirring at room temperature, make it mix fully;
(2) mixed solution of step (1) is left standstill, remove supernatant liquid and be placed on dry white solid in baking oven;
(3) by the white solid porphyrize that step (2) obtains, after being placed in retort furnace calcining, pale yellow powder is ground to obtain;
(4) pale yellow powder that step (3) obtains is scattered in NH
4hF
2stir in solution, deionized water and washing with alcohol, dry mpg-C
3n
4material.
2. the preparation method of a kind of mesoporous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (1), the cyanamide aqueous solution is 5 ~ 15 g, and nanometer colloidal silica is 10 ~ 40 g.
3. the preparation method of a kind of mesoporous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (1), churning time is 2 ~ 4 h.
4. the preparation method of a kind of mesoporous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (2), drying temperature is 40 ~ 70 DEG C.
5. the preparation method of a kind of mesoporous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (3), calcining temperature is 400 ~ 600 DEG C, and the time is 3 ~ 6 h.
6. the preparation method of a kind of mesoporous graphite phase carbon nitride material according to claim 1, is characterized in that: NH in step (4)
4hF
2the concentration of solution is 2 ~ 5 mol/L.
7. the preparation method of a kind of mesoporous graphite phase carbon nitride material according to claim 1, is characterized in that: NH in step (4)
4hF
2the consumption of solution is 300 ~ 800 mL.
8. the preparation method of a kind of mesoporous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (4), churning time is 48 ~ 64 h.
9. the preparation method of a kind of mesoporous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (4), washing times is 1 ~ 4 time.
10. the preparation method of a kind of mesoporous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (4), drying temperature is 40 ~ 70 DEG C, and the time is 1 ~ 3 h.
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Cited By (12)
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| CN105217584A (en) * | 2015-10-12 | 2016-01-06 | 济南大学 | A kind of preparation method of azotized carbon nano pipe |
| CN105879894A (en) * | 2016-04-25 | 2016-08-24 | 陕西科技大学 | (NH4)2SiF6/mpg-C3N4 powder and preparation method and application thereof |
| CN105921097A (en) * | 2016-06-01 | 2016-09-07 | 南京航空航天大学 | Preparation method and application of mesoporous graphite phase carbon nitride |
| CN106540733A (en) * | 2016-10-27 | 2017-03-29 | 太原理工大学 | A kind of method for preparing graphite phase carbon nitride material |
| CN106799250A (en) * | 2016-12-31 | 2017-06-06 | 浙江工业大学 | One species graphite-phase g C3N4/ montmorillonite composite material and its application in cellulose hydrolysis |
| CN107413364A (en) * | 2017-05-03 | 2017-12-01 | 中国科学院东北地理与农业生态研究所 | A kind of preparation method and applications of hollow mesoporous titanium dioxide of core-shell structure coated graphite phase carbon nitride composite photo-catalyst |
| CN107803216A (en) * | 2017-10-26 | 2018-03-16 | 苏州大学 | Load hollow mesoporous azotized carbon nano ball composite of bromination Nano silver grain and preparation method thereof and the application in degradation of dye |
| CN108786883A (en) * | 2018-06-07 | 2018-11-13 | 中国人民解放军陆军工程大学 | A kind of preparation method of support type ammonium perchlorate/graphene oxide three-dimensional energetic material |
| CN109701577A (en) * | 2019-01-10 | 2019-05-03 | 安徽工业大学 | A method of porous graphite phase carbon nitride is prepared using carbon nanotube as hard template |
| CN110026223A (en) * | 2019-05-07 | 2019-07-19 | 苏州十一方生物科技有限公司 | A kind of preparation method of mesoporous azotized carbon nano material |
| CN110665530A (en) * | 2019-10-16 | 2020-01-10 | 东北石油大学 | Preparation method of oxygen-doped mesoporous graphite phase carbon nitride |
| CN116371448A (en) * | 2023-05-10 | 2023-07-04 | 吉林工程技术师范学院 | Preparation method of doped mesoporous graphite phase carbon nitride |
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| CN105217584A (en) * | 2015-10-12 | 2016-01-06 | 济南大学 | A kind of preparation method of azotized carbon nano pipe |
| CN105879894B (en) * | 2016-04-25 | 2018-05-11 | 陕西科技大学 | One kind (NH4)2SiF6/mpg-C3N4Powder and its preparation method and application |
| CN105879894A (en) * | 2016-04-25 | 2016-08-24 | 陕西科技大学 | (NH4)2SiF6/mpg-C3N4 powder and preparation method and application thereof |
| CN105921097A (en) * | 2016-06-01 | 2016-09-07 | 南京航空航天大学 | Preparation method and application of mesoporous graphite phase carbon nitride |
| CN106540733A (en) * | 2016-10-27 | 2017-03-29 | 太原理工大学 | A kind of method for preparing graphite phase carbon nitride material |
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| CN106799250A (en) * | 2016-12-31 | 2017-06-06 | 浙江工业大学 | One species graphite-phase g C3N4/ montmorillonite composite material and its application in cellulose hydrolysis |
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| CN110026223A (en) * | 2019-05-07 | 2019-07-19 | 苏州十一方生物科技有限公司 | A kind of preparation method of mesoporous azotized carbon nano material |
| CN110026223B (en) * | 2019-05-07 | 2022-06-28 | 北京中科碳和科技有限公司 | Preparation method of mesoporous carbon nitride nano material |
| CN110665530A (en) * | 2019-10-16 | 2020-01-10 | 东北石油大学 | Preparation method of oxygen-doped mesoporous graphite phase carbon nitride |
| CN116371448A (en) * | 2023-05-10 | 2023-07-04 | 吉林工程技术师范学院 | Preparation method of doped mesoporous graphite phase carbon nitride |
| CN116371448B (en) * | 2023-05-10 | 2023-11-14 | 吉林工程技术师范学院 | Preparation method of doped mesoporous graphite phase carbon nitride |
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Application publication date: 20150610 |