CN105271141A - Method for preparing porous graphite-phase carbon nitride material - Google Patents
Method for preparing porous graphite-phase carbon nitride material Download PDFInfo
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- CN105271141A CN105271141A CN201510800867.XA CN201510800867A CN105271141A CN 105271141 A CN105271141 A CN 105271141A CN 201510800867 A CN201510800867 A CN 201510800867A CN 105271141 A CN105271141 A CN 105271141A
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- carbon nitride
- phase carbon
- porous graphite
- nitride material
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Abstract
The invention discloses a method for preparing a porous graphite-phase carbon nitride material. The method includes the following steps that melamine is placed in hot deionized water to be stirred till the melamine is dissolved; after the mixture is cooled to be at the indoor temperature, a HCl aqueous solution is dripped, and white precipitate is formed by stirring; after the product is dried, porous graphite-phase carbon nitride (p-g-C3N4) is obtained through calcination. The graphite-phase carbon nitride material prepared through the method is of a porous structure, and a good catalytic effect is achieved on thermal decomposition of ammonium perchlorate. According to the preparation method, the raw materials can be obtained easily, the process is simple, and product cost is lowered to a great extent; the method is suitable for industrialized mass production, and wide application prospects are achieved in the field of energetic materials.
Description
Technical field
The present invention relates to a kind of porous graphite phase carbon nitride (p-g-C
3n
4) preparation method of material, belong to material preparation and energetic material field.
Background technology
Class graphite type carbon nitride (g-C
3n
4) be allotropic substance the most stable in carbonitride, there is obvious laminate structure, in biology, catalysis and energy reserves, have good application prospect.Research shows, the catalytic effect of material and its specific surface area have close contacting.Such as, [the SuFZ such as Su, etal.CatalysisScience & Technology, 2012,2,1005] with nitrile amine for precursor power high-specific surface area carbonitride, by tBuOK and KOH solution, deprotonation is carried out to it, result shows, this material shows higher catalytic activity to Knoevenagel condensation reaction and transesterification reaction.The g-C that traditional method is prepared
3n
4specific surface area is little, inhibits its catalytic activity.Porous graphite phase carbon nitride (p-g-C can be prepared by method provided by the invention
3n
4) material, increase substantially g-C
3n
4specific surface area, effectively enhance its catalytic activity.
Ammoniumper chlorate (AP) is oxygenant conventional in solid propellant, and content accounts for 50% ~ 80% of whole formula, and the performance of its characteristic to propelling agent is most important, especially the thermal decomposition characteristic of AP and propellant burning property closely related.Therefore Study of Catalyst can estimate the catalytic effect of catalyzer to AP system propelling agent to the katalysis of AP thermolysis.Carbon material, due to its excellent performance, has been applied to ammoniumper chlorate (AP) catalytic field.Such as, king etc. [Wang Xuebao, etc. explosive wastewater journal, 2012,35,76] prepare ammoniumper chlorate/graphene aerogel (AP/GA) nano composite material by sol-gel method, the high-temperature decomposition temperature of ammoniumper chlorate is reduced 87.3 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 porous graphite phase carbon nitride (p-g-C that the present invention adopts easy method to prepare
3n
4), there is better katalysis to the thermolysis of ammoniumper chlorate (AP).
Summary of the invention
The object of this invention is to provide a kind of porous graphite phase carbon nitride (p-g-C
3n
4) preparation method of material; This method technique is simple, easy to operate, the g-C prepared with traditional method
3n
4compare, the porous graphite phase carbon nitride (p-g-C that this method is prepared
3n
4) material has larger specific surface area, thus show better catalytic effect to the thermolysis of ammoniumper chlorate.
The invention provides a kind of preparation method of porous graphite phase carbon nitride material, comprise the following steps:
(1) trimeric cyanamide is put into the deionized water of heat, stir and make it dissolve, cooling;
(2) HCl solution is added drop-wise in the solution of step (1), stirs;
(3) mixed solution that step (2) obtains is placed in oven drying, obtains white powder;
(4) white powder that step (3) obtains is placed in retort furnace calcining, calcination process for be first rapidly heated 450 ~ 500 DEG C, constant temperature 1 ~ 4h; Then be rapidly heated 500 ~ 550 DEG C, constant temperature 1 ~ 4h, obtains p-g-C
3n
4material.
In described step (1), the consumption of deionized water is 200 ~ 600ml, and Heating temperature is 70 ~ 100 DEG C, and trimeric cyanamide consumption is 10 ~ 40g.
In described step (1), churning time is 1 ~ 2h.
In described step (2), the consumption of HCl solution is 10 ~ 40ml, and volumetric molar concentration is 6 ~ 12mol/L.
In described step (2), churning time is 0.5 ~ 2h.
In described step (3), drying temperature is 50 ~ 80 DEG C, and time of drying is 12 ~ 24h.
The present invention compared with prior art, has following beneficial effect:
(1) the present invention first with hydrochloric acid and trimeric cyanamide for raw material, utilized without Template synthesis poroid class graphite phase carbon nitride p-g-C
3n
4.The present invention forms trimeric cyanamide hydrochloride by the proportioning controlling hydrochloric acid and trimeric cyanamide, and in heating polycondensation process, hydrochloric acid volatilization induced synthesis cavernous structure, avoids the poroid g-C of Template synthesis
3n
4loaded down with trivial details and the problem of environmental pollution of the building-up process caused, for synthesizing poroid g-C
3n
4provide a kind of novel method.
(2) g-C prepared with traditional method
3n
4compare, adopt p-g-C prepared by present method
3n
4there is larger specific surface area, provide active site more, accelerate electron transfer efficiency, effectively improve the activity of catalysis ammoniumper chlorate (AP) thermolysis.
(3) present method raw material is inexpensive, and preparation technology is simple, is applicable to industrialization scale operation, has very high application prospect and practical value in energetic material field.
Accompanying drawing explanation
Fig. 1 is g-C prepared by embodiment 1
3n
4with p-g-C prepared by embodiment 2
3n
4xRD curve.
Fig. 2 is p-g-C prepared by embodiment 2
3n
4fT-IR curve.
Fig. 3 is p-g-C prepared by embodiment 3
3n
4sEM picture.
Fig. 4 is p-g-C prepared by embodiment 4
3n
4tEM picture.
Fig. 5 is p-g-C prepared by embodiment 2
3n
4the performance test curve of Catalytic Performance for Decomposition of Ammonium Perchlorate.
Fig. 6 is a kind of p-g-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(comparative example)preparation g-C
3n
4
Take 5g trimeric cyanamide and put into ceramic crucible (covering crucible cover), in retort furnace, be warmed up to 500 DEG C with 50 DEG C/min, be incubated roasting 1h at this temperature, be then rapidly heated in 5min 520 DEG C, insulation roasting 1h, yellow powder sample is ground to obtain in cooling.
By material prepared by embodiment 1, after x-ray diffractometer scanning, seeing Fig. 1, is g-C
3n
4.
embodiment 2prepare poroid p-g-C
3n
4
As shown in Figure 6, a kind of preparation method of porous graphite phase carbon nitride material, comprises the following steps:
(1) taking 20g trimeric cyanamide, to be dissolved in 300ml temperature be in the deionized water of 80 DEG C, stirs 1.5h, be cooled to room temperature;
(2) be that the HCl solution of 10mol/L is added drop-wise in the solution of step (1) by 20ml concentration, stir 1h;
(3) mixed solution that step (2) obtains is placed in baking oven 60 DEG C of dry 20h, obtains white powder;
(4) white powder that step (3) obtains is placed in retort furnace calcining, calcination process for be first rapidly heated 470 DEG C, constant temperature 3h; Then be rapidly heated 510 DEG C, constant temperature 3h, finally obtain p-g-C
3n
4material.
By material prepared by embodiment 2, after x-ray diffractometer scanning, see Fig. 1, the p-g-C of preparation
3n
4with g-C prepared by usual way (embodiment 1)
3n
4the same, there is graphite-like structure.
By p-g-C prepared by embodiment 2
3n
4material, observes through Fourier transform infrared spectrometer, sees Fig. 2, poroid p-g-C
3n
4and g-C
3n
4(embodiment 1) is at 1200-1800cm
-1there is similar infrared absorption peak, show the p-g-C prepared
3n
4and g-C
3n
4the same, there is graphite-like structure.
embodiment 3prepare poroid p-g-C
3n
4
As shown in Figure 6, a kind of preparation method of porous graphite phase carbon nitride material, comprises the following steps:
(1) taking 40g trimeric cyanamide, to be dissolved in 600ml temperature be in the deionized water of 100 DEG C, stirs 1h, be cooled to room temperature;
(2) be that the HCl solution of 12mol/L is added drop-wise in the solution of step (1) by 40ml concentration, stir 1h;
(3) mixed solution that step (2) obtains is placed in baking oven 80 DEG C of dry 12h, obtains white powder;
(4) white powder that step (3) obtains is placed in retort furnace calcining, calcination process for be first rapidly heated 450 DEG C, constant temperature 4h; Then be rapidly heated 550 DEG C, constant temperature 1h, finally obtain p-g-C
3n
4material.
By p-g-C prepared by embodiment 3
3n
4material, through sem observation, is shown in Fig. 3, and the material of preparation is the p-g-C simultaneously with laminate structure and pore structure
3n
4.
embodiment 4prepare poroid p-g-C
3n
4
As shown in Figure 6, a kind of preparation method of porous graphite phase carbon nitride material, comprises the following steps:
(1) taking 10g trimeric cyanamide, to be dissolved in 200ml temperature be in the deionized water of 70 DEG C, stirs 2h, be cooled to room temperature;
(2) be that the HCl solution of 6mol/L is added drop-wise in the solution of step (1) by 10ml concentration, stir 1h;
(3) mixed solution that step (2) obtains is placed in baking oven 50 DEG C of dry 24h, obtains white powder;
The white powder that step (3) obtains is placed in retort furnace calcining, calcination process for be first rapidly heated 500 DEG C, constant temperature 1h; Then be rapidly heated 530 DEG C, constant temperature 4h, finally obtain p-g-C
3n
4material.
By p-g-C prepared by embodiment 4
3n
4material, through transmission electron microscope observation, is shown in Fig. 4, and the material of preparation is the p-g-C simultaneously with laminate structure and pore structure
3n
4.
embodiment 5p-g-C
3n
4the application of material catalyzes ammoniumper chlorate (AP) thermolysis
P-g-C prepared by Example 2
3n
4material 0.01g adds in ethanol and stirs together with 0.99g ammoniumper chlorate (AP), mixes, and after dry, sampling 9-10mg tests DTA, test condition: argon gas atmosphere, flow: 20ml/min, temperature rise rate 20 DEG C/min, temperature range: 100-500 DEG C.Test result is shown in Fig. 5, adds p-g-C
3n
4after, the high-temperature decomposition temperature of AP is 406.4 DEG C.
embodiment 6p-g-C
3n
4the application of material catalyzes ammoniumper chlorate (AP) thermolysis
P-g-C prepared by Example 2
3n
4material 0.03g adds in ethanol and stirs together with 0.97g ammoniumper chlorate (AP), mixes, and after dry, sampling 9-10mg tests DTA, test condition: argon gas atmosphere, flow: 20ml/min, temperature rise rate 20 DEG C/min, temperature range: 100-500 DEG C.Test result is shown in Fig. 5, adds p-g-C
3n
4after, the high-temperature decomposition temperature of AP is 389.2 DEG C.
embodiment 7p-g-C
3n
4the application of material catalyzes ammoniumper chlorate (AP) thermolysis
P-g-C prepared by Example 2
3n
4material 0.05g adds in ethanol and stirs together with 0.95g ammoniumper chlorate (AP), mixes, and after dry, sampling 9-10mg tests DTA, test condition: argon gas atmosphere, flow: 20ml/min, temperature rise rate 20 DEG C/min, temperature range: 100-500 DEG C.Test result is shown in Fig. 5, adds p-g-C
3n
4after, the high-temperature decomposition temperature of AP is 347.3 DEG C.
embodiment 8p-g-C
3n
4the application of material catalyzes ammoniumper chlorate (AP) thermolysis
P-g-C prepared by Example 2
3n
4material 0.1g adds in ethanol and stirs together with 0.9g ammoniumper chlorate (AP), mixes, and after dry, sampling 9-10mg tests DTA, test condition: argon gas atmosphere, flow: 20ml/min, temperature rise rate 20 DEG C/min, temperature range: 100-500 DEG C.Test result is shown in Fig. 5, adds p-g-C
3n
4after, the high-temperature decomposition temperature of AP is 342.5 DEG C.
Embodiment 5-8 result shows: along with p-g-C
3n
4addition be increased to 10wt% from 1wt%, the high-temperature decomposition temperature peak value of ammoniumper chlorate (AP) is reduced to 342.5 DEG C from 406.4 DEG C, shows the p-g-C that the present invention prepares
3n
4the thermolysis of material to ammoniumper chlorate (AP) has very strong katalysis, and ammoniumper chlorate 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 (6)
1. a preparation method for porous graphite phase carbon nitride material, is characterized in that, comprises the following steps:
(1) trimeric cyanamide is put into the deionized water of heat, stir and make it dissolve, cooling;
(2) HCl solution is added drop-wise in the solution of step (1), stirs;
(3) mixed solution that step (2) obtains is placed in oven drying, obtains white powder;
(4) white powder that step (3) obtains is placed in retort furnace calcining, calcination process for be first rapidly heated 450 ~ 500 DEG C, constant temperature 1 ~ 4h; Then be rapidly heated 500 ~ 550 DEG C, constant temperature 1 ~ 4h, obtains p-g-C
3n
4material.
2. the preparation method of a kind of porous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (1), the consumption of deionized water is 200 ~ 600ml, and Heating temperature is 70 ~ 100 DEG C, and trimeric cyanamide consumption is 10 ~ 40g.
3. the preparation method of a kind of porous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (1), churning time is 1 ~ 2h.
4. the preparation method of a kind of porous graphite phase carbon nitride material according to claim 1, is characterized in that: the consumption of the HCl solution that step (2) adds is 10 ~ 40ml, and volumetric molar concentration is 6 ~ 12mol/L.
5. the preparation method of a kind of porous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (2), churning time is 0.5 ~ 2h.
6. the preparation method of a kind of porous graphite phase carbon nitride material according to claim 1, is characterized in that: in step (3), drying temperature is 50 ~ 80 DEG C, and time of drying is 12 ~ 24h.
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Cited By (12)
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| 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 |
| CN106477539A (en) * | 2016-09-22 | 2017-03-08 | 西安交通大学 | A kind of preparation method of ultra-thin graphite phase carbon nitride |
| CN107151009A (en) * | 2017-05-09 | 2017-09-12 | 中国科学院上海硅酸盐研究所 | A kind of nitrogen-doped graphene and its preparation method and application |
| CN107352517A (en) * | 2017-07-21 | 2017-11-17 | 桂林理工大学 | A kind of preparation method of the graphite phase carbon nitride nanometer bouquet with amorphous surface |
| CN108579785A (en) * | 2018-04-20 | 2018-09-28 | 武汉工程大学 | Efficient visible light decomposes aquatic products H2Sulfur doping carbonitride preparation method |
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| CN110756209A (en) * | 2018-07-25 | 2020-02-07 | 南京理工大学 | Graphite-phase carbon nitride prepared from guanylurea nitrate and method and application thereof |
| CN110756208A (en) * | 2018-07-25 | 2020-02-07 | 南京理工大学 | Graphite-phase carbon nitride material for catalytic reduction of p-nitrophenol and preparation method and application thereof |
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| US20200269222A1 (en) * | 2016-02-16 | 2020-08-27 | The George Washington University | Doped graphitic carbon nitrides, methods of making and uses of the same |
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| US11850575B2 (en) * | 2016-02-16 | 2023-12-26 | The George Washington University | Doped graphitic carbon nitrides, methods of making and uses of the same |
| 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 |
| 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 |
| CN106477539B (en) * | 2016-09-22 | 2019-03-01 | 西安交通大学 | A kind of preparation method of ultra-thin graphite phase carbon nitride |
| CN106477539A (en) * | 2016-09-22 | 2017-03-08 | 西安交通大学 | A kind of preparation method of ultra-thin graphite phase carbon nitride |
| CN107151009A (en) * | 2017-05-09 | 2017-09-12 | 中国科学院上海硅酸盐研究所 | A kind of nitrogen-doped graphene and its preparation method and application |
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| CN107352517A (en) * | 2017-07-21 | 2017-11-17 | 桂林理工大学 | A kind of preparation method of the graphite phase carbon nitride nanometer bouquet with amorphous surface |
| CN108579785B (en) * | 2018-04-20 | 2021-10-12 | 武汉工程大学 | High-efficiency visible light decomposition aquatic product H2Preparation method of sulfur-doped carbon nitride |
| CN108579785A (en) * | 2018-04-20 | 2018-09-28 | 武汉工程大学 | Efficient visible light decomposes aquatic products H2Sulfur doping carbonitride preparation method |
| CN108671956A (en) * | 2018-05-31 | 2018-10-19 | 武汉大学 | A kind of preparation method of ion filled graphite phase carbon nitride nanometer sheet |
| CN108671956B (en) * | 2018-05-31 | 2021-04-02 | 武汉大学 | Preparation method of ion-filled graphite-phase carbon nitride nanosheet |
| CN110756209A (en) * | 2018-07-25 | 2020-02-07 | 南京理工大学 | Graphite-phase carbon nitride prepared from guanylurea nitrate and method and application thereof |
| CN110756208A (en) * | 2018-07-25 | 2020-02-07 | 南京理工大学 | Graphite-phase carbon nitride material for catalytic reduction of p-nitrophenol and preparation method and application thereof |
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