CN113060710B - Method for extracting graphite-phase carbon nitride from coal gangue - Google Patents
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- C01B21/00—Nitrogen; Compounds thereof
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Abstract
The invention provides a method for extracting graphite-phase carbon nitride from coal gangue minerals, which comprises the following steps: selecting coal gangue with different volatile component contents as raw materials, and blending to ensure that the mass ratio of carbon element to nitrogen element in volatile components in the coal gangue is 1: 1-2; roasting the prepared coal gangue for 1-100min under the pyrolysis atmosphere and at the temperature of 700-900 ℃; rapidly cooling the roasted coal gangue to 20-400 ℃ at a cooling rate of more than 15 ℃/min, and then preserving heat for 1-2h to obtain the graphite-phase carbon nitride film. The method for extracting the graphite-phase carbon nitride from the coal gangue, provided by the invention, can realize rapid, efficient and large-scale preparation of the graphite-phase carbon nitride material, can realize recovery of valuable elements in the coal gangue, and responds to the national policy of solid waste recycling.
Description
Technical Field
The invention relates to the technical field of extraction of valuable substances in coal gangue minerals, in particular to a method for extracting graphite-phase carbon nitride from coal gangue.
Background
Carbon nitride (C) 3 N 4 ) The compound does not exist in nature, needs artificial synthesis, has the advantages of low density, high chemical stability, good biocompatibility, strong wear resistance and the like, has wide application prospect in the fields of high-performance wear-resistant coatings, membrane materials, catalysts and catalyst carriers, preparation of metal nitrides, blue-light emitting materials or high-temperature semiconductor materials and the like, and is widely concerned by people for a long time 3 N 4 ) The theory and experiment of material preparation have made great progress, and the synthesis of alpha-C is reported 3 N 4 、β-C 3 N 4 Graphite phase or CNx, etc.
The existing preparation method of carbon nitride mainly adopts the preparation methods of a chemical vapor deposition method, an ion beam sputtering method, laser plasma deposition and laser ablation, ion plating, an ion implantation method and the like. However, the problems generally faced by the method are that the preparation is difficult, the energy consumption is high, the yield is low and the like, a new idea needs to be found for the mass preparation of the carbon nitride material, and the problems that the preparation process flow is complicated, the consumed time is long, the energy is more, the efficiency is low, the industrial mass production is not facilitated and the like are solved.
The coal gangue is rich in elements such as carbon, silicon, aluminum, nitrogen and the like, but the coal gangue is generally stacked on a mine as waste stones, the stacking amount is increased day by day, and billions of tons of stacking amount exist at present, which has influence on environmental protection, so that a method for extracting carbon and nitrogen elements from the coal gangue is sought, and the method has great significance.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for extracting graphite-phase carbon nitride from coal gangue, which not only can realize rapid, efficient and large-scale preparation of graphite-phase carbon nitride materials, but also can realize recovery of valuable elements in coal gangue, and respond to the national policy of solid waste recycling.
In order to achieve the aim, the invention provides a method for extracting graphite-phase carbon nitride from coal gangue, which comprises the following steps:
step one, selecting coal gangue with different volatile component contents as raw materials, and blending to enable the mass ratio of carbon element to nitrogen element in volatile components in the coal gangue to be 1: 1-2;
step two, placing the coal gangue prepared in the step one into a closed crucible to be roasted for 1-100min under the pyrolysis atmosphere and at the temperature of 700-;
and step three, rapidly cooling the closed crucible filled with the roasted coal gangue to 20-400 ℃ at a cooling rate of more than 15 ℃/min, and then preserving heat for 1-2h, namely depositing a graphite phase carbon nitride film on the inner surface of the crucible.
Further, the components of the coal gangue in the first step comprise moisture, ash, volatile matters and fixed carbon.
Further, the moisture includes physically adsorbed water and chemically bound water; the ash comprises silicon dioxide and aluminum oxide; the volatile matter comprises organic matters formed by carbon elements, hydrogen elements, oxygen elements and nitrogen elements.
Further, the coal gangue raw material in the first step comprises, by mass, 1% -15% of water, 40% -95% of ash, 1% -50% of volatile matter and 1% -50% of fixed carbon.
Further, the content of carbon in organic matters in the volatile matters in the coal gangue is measured by TOC, and the content of nitrogen is measured by BOD.
Further, in the second step, the pyrolysis atmosphere is any one of nitrogen, argon, air and vacuum conditions.
Further, the time of the rapid cooling process in the third step is 1-60 min.
Further, the coal gangue prepared in the step two is placed on a heat-resistant carrier, and the heat-resistant carrier is a quartz crucible or a ceramic crucible.
Further, the thickness of the graphite phase carbon nitride film is 0.001-1 mm.
The invention has the following beneficial effects:
the invention provides a method for extracting graphite-phase carbon nitride from coal gangue, which comprises the steps of firstly combining coal gangue in different producing areas, adjusting the carbon-nitrogen ratio, ensuring an enough raw material ratio, then roasting at a high temperature for a short time to generate a chemical combination reaction, combining carbon with nitrogen to generate carbon nitride molecules, then rapidly cooling to ensure that gaseous carbon nitride is rapidly condensed and deposited on the inner surface of a crucible, if slowly cooling, most of carbon nitride exists in gaseous molecules, the tightness is not tight, most of carbon nitride volatilizes in gaseous state, the deposition or deposition amount is small, and finally keeping the temperature at a low temperature of about 20-400 ℃ for 1-2h to ensure the stable deposition and slow growth of carbon nitride on the inner surface of the crucible to reach a certain thickness. The method for extracting the graphite-phase carbon nitride from the coal gangue, provided by the invention, can realize rapid, efficient and large-scale preparation of the graphite-phase carbon nitride material, can realize recovery of valuable elements in the coal gangue, and responds to the national policy of solid waste recycling.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of a process for extracting graphite-phase carbon nitride from coal gangue in accordance with the present invention;
FIG. 2 is an XRD pattern of graphite phase carbon nitride produced in accordance with preferred embodiment 5 of the present invention;
FIG. 3 is a pictorial view of a graphite phase carbon nitride produced in accordance with preferred embodiment 5 of the present invention;
FIG. 4 is a pictorial representation of graphite phase carbon nitride prepared in comparative example 1 of the present invention;
FIG. 5 is a pictorial representation of a graphite phase carbon nitride prepared in comparative example 2 of the present invention.
Detailed Description
Embodiments of the invention will be described in detail below with reference to the drawings, but the invention can be implemented in many different ways, which are defined and covered by the claims.
The method aims at utilizing the coal gangue, so that raw materials are produced from different regions including Ningxia, Ordos, Shanxi, Henan and the like, the raw material components of the coal gangue in each region are greatly different, the volatile component contents in the coal gangue in different regions are different, the specific carbon-nitrogen ratio is high or low, and the ideal carbon nitride film is prepared by adjusting the proper carbon content through mutual matching.
The components of the raw material coal gangue comprise moisture, ash content, volatile matter and fixed carbon. The coal gangue raw material comprises, by mass, 1% -15% of water, 40% -95% of ash, 1% -50% of volatile matter and 1% -50% of fixed carbon. Coal gangue in different producing areas has different components, ash content is 40-95%, and the main component of ash content is SiO 2 And Al2O 3 The silicon-aluminum ratio is 0.6-1.4. The volatile components being mainly organic compounds of carbon, hydrogen, oxygen, nitrogen, e.g. CH 4 Equal CH compound, CH oxide, HCN, NH 3 And nitrogen-containing organic compounds. The coal gangue in different producing areas has large water difference, the water content is 1 to 15 percent, and the coal gangue comprises physical adsorption water and chemical binding water.
The carbon and nitrogen elements participating in the reaction are all derived from organic matters in volatile matters, and do not relate to fixed carbon in the coal gangue, because the preparation process is very fast, and the fixed carbon cannot react in time due to the closed space and still exists in the coal gangue. Therefore, the adjustment of the carbon-nitrogen ratio is independent of the fixed carbon content difference of different raw materials and only depends on the content of organic matters in volatile matters, and the carbon-nitrogen ratio of the organic matters in the specific volatile matters is measured by BOD and TOC. The content of carbon element in the organic matters in the volatile matters in the coal gangue is measured by TOC, and the content of nitrogen element is measured by BOD. For example, the initial raw material selects the coal gangue in the Ordos producing area, the carbon-nitrogen ratio is close to 1:1, and the carbon-nitrogen ratio can be adjusted by combining the coal gangue in different producing areas.
As shown in fig. 1, the invention provides a method for extracting graphite-phase carbon nitride from coal gangue, which comprises the following steps:
step one, selecting coal gangue with different volatile component contents as raw materials, and blending to enable the mass ratio of carbon element to nitrogen element in volatile components in the coal gangue to be 1: 1-2;
step two, placing the coal gangue prepared in the step one into a closed crucible to be roasted for 1-100min under the pyrolysis atmosphere and at the temperature of 700-;
and step three, rapidly cooling the closed crucible filled with the roasted coal gangue to 20-400 ℃ at a cooling rate of more than 15 ℃/min, and then preserving heat for 1-2h, namely depositing a graphite phase carbon nitride film on the inner surface of the crucible.
The invention firstly combines coal gangue in different producing areas, adjusts the carbon-nitrogen ratio, ensures sufficient raw material ratio, then is roasted for a short time at high temperature to generate chemical combination carbon-nitrogen combination to generate carbon nitride molecules, then is rapidly cooled to ensure that gaseous carbon nitride is rapidly condensed and deposited on the inner surface of the crucible, if the carbon nitride is slowly cooled, most of the carbon nitride exists in gaseous molecules, the tightness is not tight, most of the carbon nitride volatilizes in gaseous state, the carbon nitride can not be deposited or the deposition amount is small, and finally, the temperature is kept for 1-2h at low temperature of about 20-400 ℃, the stable deposition of the carbon nitride and the slow growth on the inner surface of the crucible are ensured, and a certain thickness is reached. The method for extracting the graphite-phase carbon nitride from the coal gangue, provided by the invention, can realize rapid, efficient and large-scale preparation of the graphite-phase carbon nitride material, can realize recovery of valuable elements in the coal gangue, and responds to the national policy of solid waste recycling.
Example 1
A method for extracting graphite-phase carbon nitride from coal gangue comprises the following steps:
firstly, selecting coal gangue with different volatile component contents as a raw material, testing the contents of moisture, ash, volatile components and fixed carbon in coal gangue minerals, and adjusting the carbon-nitrogen ratio in the volatile components to be 1: 1.5, roasting at 800 ℃ for 15min under a closed vacuum condition, taking out from the furnace, placing in a heat preservation box at 100 ℃, preserving heat for 1h, and forming a layer of graphite phase carbon nitride film with uniform texture on the inner surface of the crucible.
Example 2
A method for extracting graphite-phase carbon nitride from coal gangue comprises the following steps:
firstly, selecting coal gangue with different volatile component contents as a raw material, testing the contents of moisture, ash, volatile components and fixed carbon in coal gangue minerals, and adjusting the carbon-nitrogen ratio in the volatile components to be 1:1, roasting at 800 ℃ for 15min under a closed vacuum condition, taking out from the furnace, placing in a heat preservation box at 100 ℃, preserving heat for 1h, and forming a layer of graphite phase carbon nitride film with uniform texture on the inner surface of the crucible.
Example 3
A method for extracting graphite-phase carbon nitride from coal gangue comprises the following steps:
firstly, selecting coal gangue with different volatile component contents as a raw material, testing the contents of moisture, ash, volatile components and fixed carbon in coal gangue minerals, and adjusting the carbon-nitrogen ratio in the volatile components to be 1: 2, roasting at 800 ℃ for 15min under a closed vacuum condition, taking out from the direct furnace, placing in a heat preservation box at 100 ℃, preserving heat for 1h, and forming a layer of graphite phase carbon nitride film with uniform texture on the inner surface of the crucible.
Example 4
A method for extracting graphite-phase carbon nitride from coal gangue comprises the following steps:
firstly, selecting coal gangue with different volatile component contents as a raw material, testing the contents of moisture, ash, volatile components and fixed carbon in coal gangue minerals, and adjusting the carbon-nitrogen ratio in the volatile components to be 1: 1.5, roasting at 700 ℃ for 15min under a closed vacuum condition, taking out from the furnace, placing in a heat preservation box at 100 ℃, preserving heat for 1h, and forming a layer of graphite phase carbon nitride film with uniform texture on the inner surface of the crucible.
Example 5
A method for extracting graphite-phase carbon nitride from coal gangue comprises the following steps:
firstly, selecting coal gangue with different volatile component contents as a raw material, testing the contents of moisture, ash, volatile components and fixed carbon in coal gangue minerals, and adjusting the carbon-nitrogen ratio in the volatile components to be 1: 1.5, then roasting at 900 ℃ for 15min under the closed vacuum condition, then taking out from the furnace, placing in a heat preservation box at 100 ℃, and preserving heat for 1h, wherein a layer of graphite phase carbon nitride film with uniform texture is formed on the inner surface of the crucible (as shown in figure 3). Example 5 is a preferred experiment for this experiment.
Fig. 2 is an X-ray diffraction pattern of the graphite-phase carbon nitride film obtained in example 5, and by analyzing and testing characteristic diffraction peaks appearing at 13.11 ° and 27.4 ° in the XRD diffraction pattern, the diffraction peaks respectively correspond to the (100) crystal plane stacked between the crystal planes of the graphite-phase carbon nitride and the (002) crystal plane stacked between the layers, which proves that the carbon nitride prepared by the method is graphite-phase carbon nitride.
Comparative example 1: (Slow Cooling)
A method for extracting graphite-phase carbon nitride from coal gangue comprises the following steps:
firstly, selecting coal gangue with different volatile component contents as a raw material, testing the contents of moisture, ash, volatile components and fixed carbon in coal gangue minerals, and adjusting the carbon-nitrogen ratio in the volatile components to be 1: 1.5, roasting at 800 ℃ for 15min under a closed vacuum condition, cooling along with the furnace to be slowly cooled to 100 ℃ (the cooling speed is far less than 15 ℃/min), preserving heat for 1h, forming a very incomplete graphite phase carbon nitride film on the inner surface of the crucible at the moment, having serious fracture defects, no carbon nitride deposition in many places and having obvious and quick cooling effect (as shown in figure 4).
The main reason is that the cooling speed is too slow, the gaseous nitride can not be rapidly condensed and deposited on the surface of the crucible, most of the gaseous nitride is volatilized, the formed carbon nitride film is incomplete, and the strength is poor.
Therefore, in order to ensure that carbon nitride with a certain thickness is produced, rapid cooling is required, namely the carbon nitride is heated at the temperature of about 900 ℃, is rapidly taken out and is placed into a drying oven at the temperature of 100 ℃ for air cooling and cooling, the temperature is reduced to 100 ℃ for one hour, and the cooling rate of rapid cooling is required to be more than 15 ℃/min.
Comparative example 2: (too low carbon to nitrogen ratio in volatile)
Comparative example 2 differs from the examples in that: in comparative example 2, the carbon-nitrogen ratio in the volatile components was adjusted to 1: 0.8, the rest is the same as example 1.
In comparative example 2, a graphite phase carbon nitride film having a uniform texture was formed on the inner surface of the crucible, but the thickness was very thin (as shown in FIG. 5).
The main reasons are that the carbon content is insufficient, the carbon-nitrogen ratio of the theoretical carbon nitride is not reached, the generated carbon nitride is less, and the film thickness is insufficient.
Comparative example 3: (too high ratio of carbon to nitrogen in volatile)
Comparative example 3 differs from the examples in that: in comparative example 3, the carbon-nitrogen ratio in the volatile components was adjusted to 1: 2.2, the rest is the same as example 1.
In comparative example 3, a graphite phase carbon nitride film having a uniform texture was formed on the inner surface of the crucible, but the thickness was very thin.
The main reason is that when the content of nitrogen in the volatile matter is too high, the other volatile matter of nitrogen inhibits the generation of carbon nitride, and the film thickness is not sufficient.
Comparative example 4: (baking temperature is too low)
Comparative example 4 differs from the examples in that: the calcination temperature in comparative example 4 was 650 ℃ as in example 1.
In comparative example 4, an incomplete graphite-phase carbon nitride film was formed on the inner surface of the crucible, and the defect was serious.
The main reasons are that the temperature is too low, the reactivity of carbon and nitrogen atoms is insufficient, the combination is too weak, and the strength of the generated film is insufficient and incomplete.
Comparative example 5: (calcination temperature too high)
Comparative example 5 differs from the examples in that: the calcination temperature in comparative example 5 was 650 ℃ as in example 1.
In comparative example 5, a graphite phase carbon nitride film having a uniform texture was formed on the inner surface of the crucible, but the thickness was very thin.
The main reason is that when the temperature is too high, part of carbon and nitrogen forms other compounds and is volatilized, so that the generation amount of carbon nitride is small and the film thickness is insufficient.
In conclusion, the key parameters of the preparation method of the invention are as follows: the ratio of carbon to nitrogen in volatile components is 1: 1.5 to 1: 2 and the roasting temperature is 700-900 ℃, and the carbon nitride film prepared by rapid cooling has uniform texture, good stability and considerable thickness. Because 700-900 ℃ is favorable for the growth of lamellar graphite phase carbon nitride structure, the reaction activity between nitrogen and carbon atoms is insufficient and the combination is too little when the temperature is too low, the structure of graphite phase is damaged when the temperature is too high, the carbon-nitrogen ratio is 1: 1.5 is the demand ratio of theoretical carbon nitride molecules, too low is not enough for forming carbon nitride, and in practice, the nitrogen content is slightly more favorable for the growth of a carbon nitride film, but not too high, and the reaction is inhibited, 1: 1.5 to 1: 2 the conditions are optimal.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for extracting graphite-phase carbon nitride from coal gangue is characterized by comprising the following steps:
step one, selecting coal gangue with different volatile component contents as raw materials, and blending to enable the mass ratio of carbon element to nitrogen element in volatile components in the coal gangue to be 1: 1-2;
step two, placing the coal gangue prepared in the step one into a closed crucible to be roasted for 1-100min under the pyrolysis atmosphere and at the temperature of 700-;
and step three, rapidly cooling the closed crucible filled with the roasted coal gangue to 20-400 ℃ at a cooling rate of more than 15 ℃/min, and then preserving heat for 1-2h, namely depositing a graphite phase carbon nitride film on the inner surface of the crucible.
2. The method for extracting graphite-phase carbon nitride from coal gangue as claimed in claim 1, wherein the components of the coal gangue in the first step comprise moisture, ash, volatile matters and fixed carbon.
3. The method for extracting graphite-phase carbon nitride from coal gangue as claimed in claim 2, wherein the water comprises physically adsorbed water and chemically bound water; the ash comprises silicon dioxide and aluminum oxide; the volatile matter comprises organic matters formed by carbon elements, hydrogen elements, oxygen elements and nitrogen elements.
4. The method for extracting graphite-phase carbon nitride from coal gangue as claimed in claim 2, wherein the coal gangue raw material in the first step comprises, by mass, 1% -15% of water, 40% -95% of ash, 1% -50% of volatile matter, and 1% -50% of fixed carbon.
5. The method for extracting graphite-phase carbon nitride from coal gangue as claimed in claim 3, wherein the content of carbon in the organic matter in the volatile matter in the coal gangue is measured by TOC and the content of nitrogen is measured by BOD.
6. The method for extracting graphite-phase carbon nitride from coal gangue as claimed in any one of claims 1-5, wherein the pyrolysis atmosphere in the second step is any one of nitrogen, argon, air and vacuum conditions.
7. The method for extracting graphite-phase carbon nitride from coal gangue as claimed in any one of claims 1 to 5, wherein the time of the rapid cooling process in the third step is 1-60 min.
8. The method for extracting graphite-phase carbon nitride from coal gangue as claimed in claim 1, wherein the thickness of the graphite-phase carbon nitride film is 0.001-1 mm.
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