CN111825067A - Preparation method of cellular nano carbon nitride and application of cellular nano carbon nitride - Google Patents
Preparation method of cellular nano carbon nitride and application of cellular nano carbon nitride Download PDFInfo
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- CN111825067A CN111825067A CN202010704605.4A CN202010704605A CN111825067A CN 111825067 A CN111825067 A CN 111825067A CN 202010704605 A CN202010704605 A CN 202010704605A CN 111825067 A CN111825067 A CN 111825067A
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Abstract
The invention relates to a preparation method of honeycomb-shaped nanometer carbon nitride and application of the honeycomb-shaped nanometer carbon nitride, which comprises the following steps: placing urea in a covered crucible, carrying out programmed heating in a muffle furnace for primary calcination, grinding after cooling, placing the urea in the covered crucible again, carrying out programmed heating in the muffle furnace for secondary calcination, and obtaining the honeycomb-shaped nano carbon nitride after cooling; the programmed heating rate of the first calcination is 10-20 ℃/min; the temperature of the first calcination is 500-600 ℃, and the heat preservation time is 1-6 h; the temperature programming rate of the second calcination is 10-15 ℃/min; the temperature of the second calcination is 490-560 ℃, and the heat preservation time is 1-10 h. The honeycomb-shaped nanometer carbon nitride prepared by the method has larger specific surface area and pore volume, and has higher adsorption capacity and removal rate for lead ions.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of honeycomb-shaped nano carbon nitride and application of the honeycomb-shaped nano carbon nitride.
Background
Heavy metal pollution can cause plant withering, air pollution and death of organisms in water, and if the heavy metal pollution enters a human body, the heavy metal pollution can cause damage to the human body and can cause death in serious cases. Heavy metal pollution in wastewater is widely concerned by scholars at home and abroad due to the characteristics of bioaccumulation, high toxicity, easy carcinogenesis and the like. Heavy metal ions such as copper, lead, chromium and the like are typical heavy metal pollutants in wastewater. At present, several technologies are used for treating heavy metals in wastewater, such as neutralization method, ion exchange method, sulfuration method, etc., however, the above methods all have disadvantages, such as the ion exchange method has a great limitation in its application due to its expensive resin cost and regeneration cost; the membrane separation method has high treatment efficiency, but has high cost and complex operation; the chemical precipitation method is accompanied with the generation of a large amount of sludge in the treatment process. The adsorption method can be used for treating various kinds of wastewater containing heavy metals, and particularly has higher treatment efficiency for low-concentration wastewater containing heavy metals.
The graphite phase carbon nitride material has good chemical stability, good biocompatibility and high hardness, and the material has the characteristics of small average pore diameter, more concentrated pore channel structure, high porosity and narrow pore diameter distribution, has the characteristics of short distance, namely disordered atomic level, and long distance, namely ordered mesoscopic level in the structure, and shows good potential in the aspect of adsorbing heavy metal ions in water. However, the common graphite phase carbon nitride is limited by the specific surface area and the pore volume, so that the carbon nitride has a small adsorption amount when being used as a heavy metal ion adsorbent, and too small pore volume can only contain less metal ions, thereby greatly limiting the adsorption capacity of the carbon nitride. So that the modification treatment is particularly important.
In the prior art, raw materials such as melamine are directly roasted to obtain carbon nitride, and the material is utilized to adsorb Pb2+Prepared carbon nitride to Pb2+The maximum adsorption capacity is 7.4mg/g, and the carbon nitride prepared by direct calcination adsorbs Pb2+There is a problem that the adsorption amount is too small. Also, porous carbon nitride prepared by adding pore-expanding agent such as lithium chloride into raw materials such as melamine and the like and used for adsorbing Pb2+The maximum adsorption capacity can reach 28.6 mg/g. Also uses thiourea as the starting material to prepare graphite phase carbon nitride by template-free method, which is opposite to Pb2+The maximum adsorption amount of the catalyst is 65.6mg/g, although the graphite-phase carbon nitride prepared by the thiourea template-free method adsorbs Pb2+The amount is high, but the graphite phase carbon nitride prepared by the template-free method still has the problems of small specific surface area and small pore volume.
Disclosure of Invention
In order to solve the problem of small lead ion adsorption capacity caused by the technical problem of small specific surface area and pore volume of common graphite-phase carbon nitride in the prior art, a preparation method of honeycomb-shaped nano carbon nitride and application of the honeycomb-shaped nano carbon nitride are provided. The structure of the nano carbon nitride prepared by the method is honeycomb-shaped, and has larger specific surface area and pore volume, and the honeycomb-shaped nano carbon nitride has higher adsorption capacity and removal rate to lead ions in water environment.
The invention provides a preparation method of honeycomb-shaped nanometer carbon nitride, which comprises the following steps: and (3) placing the urea in a covered crucible, carrying out programmed heating in a muffle furnace for primary calcination, grinding after cooling, placing in the covered crucible again, carrying out programmed heating in the muffle furnace for secondary calcination, and cooling to obtain the honeycomb-shaped nano carbon nitride. The use of a covered crucible during the calcination process is to make the N element released by the urea under high temperature conditions remain in the product to obtain carbon nitride; the second calcination after grinding is performed in order to uniformly heat the product during the second calcination.
Further, the temperature programming rate of the first calcination is 10-20 ℃/min; the temperature of the first calcination is 500-600 ℃, and the heat preservation time is 1-6 h.
Preferably, the temperature programming rate of the first calcination is 10 ℃/min; the temperature of the first calcination is 550 ℃, and the heat preservation time is 3 h.
Further, the temperature programming rate of the second calcination is 10-15 ℃/min; the temperature of the second calcination is 490-560 ℃, and the heat preservation time is 1-10 h.
Preferably, the temperature programming rate of the second calcination is 10 ℃/min; the temperature of the second calcination is 520 ℃, and the heat preservation time is 4 h.
The invention also provides a method for preparing the honeycomb-shaped nano carbon nitride by using the method.
Further, the conditions of the application are: the temperature is 30 ℃, the pH value of the water environment containing lead ions is adjusted to be 3, and 0.4g/L of the honeycomb-shaped nano carbon nitride is added to adsorb the lead ions in the water environment for 1.5 h.
The beneficial technical effects are as follows:
the invention prepares the cellular nano carbon nitride by secondary calcination, the prepared cellular nano carbon nitride has larger specific surface area and pore volume, the adsorption capacity to lead ions is improved, and the cellular nano carbon nitride prepared by the method has obvious adsorption effect to the lead ions. The invention directly uses cheap urea as raw material, the source of the needed raw material is rich, the preparation process is simple and convenient to operate, the cost is low, and no secondary pollution is caused.
Drawings
Fig. 1 is a scanning electron microscope image of the honeycomb-shaped nano carbon nitride prepared in example 1 of the present invention.
FIG. 2 is a scanning electron microscope photograph of graphite-phase carbon nitride obtained after the first calcination in example 1 of the present invention.
FIG. 3 is the present inventionIllustrating the BET data of the first calcined product graphitic carbon nitride and the second calcined product cellular carbon nitride in comparison of example 1, wherein (a) is a BJH pore size distribution plot, and (b) is N2Adsorption-desorption isotherm diagram.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
It should be noted that the words "first", "second", etc. are used to define the order of calcination, and are only used for convenience of distinguishing the order of the calcination process, and the words have no special meaning unless otherwise stated, and therefore, should not be construed as limiting the scope of the present invention.
Example 1
A preparation method of honeycomb-shaped nanometer carbon nitride comprises the following steps:
and (2) putting 10g of urea into a covered crucible, then putting the crucible into a muffle furnace, raising the temperature to 550 ℃ at the heating rate of 10 ℃/min, then preserving the heat for 3h, naturally cooling, then taking out the graphite-phase carbon nitride, grinding, putting the crucible into the covered crucible again, then putting the crucible into the muffle furnace, raising the temperature to 520 ℃ at the heating rate of 10 ℃/min, preserving the heat for 4h, naturally cooling, then taking out the ground, and cooling to obtain the honeycomb-shaped nano carbon nitride.
The morphology of the graphite phase carbon nitride obtained by the first calcination is observed by a scanning electron microscope, and an SEM image is shown in fig. 2, and it can be seen from fig. 2 that the morphology of the graphite phase carbon nitride is lamellar stacking.
The morphology of the product obtained by calcining the graphite-phase carbon nitride for the first time and then calcining the graphite-phase carbon nitride for the second time is observed by a scanning electron microscope, the SEM image is shown in figure 1, and as can be seen from figure 1, the morphology of the graphite-phase carbon nitride obtained by calcining for the first time is changed by calcining for the second time, and the graphite-phase carbon nitride is changed into a honeycomb shape from sheet accumulation.
BET test results of the graphite-phase carbon nitride obtained by the first calcination and the cellular carbon nitride obtained by the second calcination are shown in FIG. 3, in which (a) is a BJH pore size distribution diagram and (b) is N2Adsorption-desorption isotherm diagram. As can be seen from FIG. 3, the graphite-phase carbon nitride obtained by the first calcination had a pore diameter of 2.58nm and a specific surface area of 129.210m2·g-1The aperture of the cellular nano carbon nitride prepared by the second calcination is 2.88nm, and the specific surface area is 153.109m2·g-1. The pore diameter, specific surface area and pore volume data of both are shown in Table 1.
TABLE 1 pore size, specific surface area and pore volume data for the twice calcined product
As can be seen from fig. 3 and table 1, the specific surface area and pore volume of the honeycomb-shaped nano carbon nitride prepared by re-calcination are both increased to a certain extent, which can effectively improve the adsorption capacity of the honeycomb-shaped nano carbon nitride to heavy metal ions.
Example 2
The preparation method of the honeycomb-shaped nano carbon nitride is the same as that of the embodiment 1, except that: the temperature rise rate of the first calcination is 15 ℃/min; the holding time of the second calcination is 5 h.
Example 3
The preparation method of the honeycomb-shaped nano carbon nitride is the same as that of the embodiment 1, except that: the heating rate of the first calcination is 20 ℃/min; the holding time of the second calcination is 5 h.
Example 4
The preparation method of the honeycomb-shaped nano carbon nitride is the same as that of the embodiment 1, except that: the temperature of the first calcination is 500 ℃; the holding time of the second calcination is 5 h.
Example 5
The preparation method of the honeycomb-shaped nano carbon nitride is the same as that of the embodiment 1, except that: the holding time of the second calcination is 5 h.
Example 6
The preparation method of the honeycomb-shaped nano carbon nitride is the same as that of the embodiment 1, except that: the temperature rising rate of the second calcination is 15 ℃/min, and the heat preservation time is 3 h.
Example 7
The preparation method of the honeycomb-shaped nano carbon nitride is the same as that of the embodiment 1, except that: the temperature of the second calcination is 560 ℃, and the holding time is 2 h.
Comparative example 1
The preparation method of the nano carbon nitride of the present comparative example is the same as that of example 1 except that: the heating rate of the first calcination is 5 ℃/min; the holding time of the second calcination is 5 h.
Comparative example 2
The preparation method of the nano carbon nitride of the present comparative example is the same as that of example 1 except that: the temperature of the first calcination is 500 ℃; the temperature of the second calcination is 480 ℃, and the heat preservation time is 5 h.
The preparation conditions and the product morphology of the above examples and comparative examples are shown in Table 2.
TABLE 2 preparation conditions and product morphology for the examples and comparative examples
From the above examples, it can be seen that the condition of the first calcination has little influence on the morphology of the product, and the mechanism of the second calcination to form the honeycomb-shaped nano carbon nitride may be: after the graphite phase carbon nitride is formed by primary calcination, certain dislocation is generated between graphite phase carbon nitride layers through grinding, acting force between molecules is weakened, and the graphite phase carbon nitride layers which generate the dislocation are curled under the influence of secondary calcination mainly on secondary calcination temperature, so that a honeycomb shape is formed.
Application example 1
The carbon nitride prepared in the above examples and comparative examples was applied to adsorb lead ions in an aqueous environment.
Respectively adding 8mg of the honeycomb-shaped nano carbon nitride in the embodiments 1 to 7 into 20mL of the mixture and 50mg/L of the mixture containing Pd2+After completion of the adsorption, the adsorbed solution was centrifuged (3000r/min, 5min), and the supernatant was collected and the Pb in the supernatant after the adsorption was measured with a flame atomic absorption spectrophotometer2+Then the concentration of the prepared honeycomb nano carbon nitride to Pd in each example is calculated2+The data of the removal rate are shown in Table 3.
TABLE 3 prepared in the examples and comparative examples
As can be seen from Table 3, the cellular carbon nitride nanoparticles of the present invention have a high Pb content2+Has good adsorption capacity to Pb2+The adsorption capacity can reach 114.2mg/g at most, and the removal rate reaches 91.2%. The honeycomb-shaped nanometer carbon nitride has larger aperture and specific surface area, and the adsorption capacity of the honeycomb-shaped nanometer carbon nitride to metal ions is improved.
The graphite-phase carbon nitride obtained after the first calcination and the cellular carbon nitride obtained after the second calcination in example 1 were recovered, and Pb was removed with 0.1mol/L NaOH solution2+Washing bees with metal ions and deionized waterThe cellular carbon nitride was dried to neutrality and reused 10 times according to the above method, and the results are shown in table 4.
TABLE 4 results after 10-fold reuse
As can be seen from Table 4, the cellular carbon nitride obtained after the second calcination of the present invention has greatly improved Pb content compared to the graphite-phase carbon nitride obtained after the first calcination2+And for Pb after 10 times of repeated use2+The removal rate of (D) was still 83.4%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. A preparation method of honeycomb-shaped nanometer carbon nitride is characterized by comprising the following steps:
placing urea in a covered crucible, carrying out programmed heating in a muffle furnace for primary calcination, grinding after cooling, placing the urea in the covered crucible again, carrying out programmed heating in the muffle furnace for secondary calcination, and obtaining the honeycomb-shaped nano carbon nitride after cooling;
the programmed heating rate of the first calcination is 10-20 ℃/min; the temperature of the first calcination is 500-600 ℃, and the heat preservation time is 1-6 h;
the temperature programming rate of the second calcination is 10-15 ℃/min; the temperature of the second calcination is 490-560 ℃, and the heat preservation time is 1-10 h.
2. The method for preparing honeycomb nano carbon nitride according to claim 1, wherein the temperature programming rate of the first calcination is 10 ℃/min; the temperature of the first calcination is 550 ℃, and the heat preservation time is 3 h.
3. The method for preparing honeycomb nano carbon nitride according to claim 1, wherein the temperature programming rate of the second calcination is 10 ℃/min; the temperature of the second calcination is 520 ℃, and the heat preservation time is 4 h.
4. The honeycomb-shaped nano carbon nitride prepared by the preparation method according to any one of claims 1 to 3 is applied to adsorption of lead ions in water environment.
5. The application according to claim 4, characterized in that the conditions of the application are: the temperature is 30 ℃, the pH value of the water environment containing lead ions is adjusted to be 3, and 0.4g/L of the honeycomb-shaped nano carbon nitride is added to adsorb the lead ions in the water environment for 1.5 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113086955A (en) * | 2021-03-30 | 2021-07-09 | 武汉大学 | Preparation method of carbon-deficient carbon nitride material for photocatalytic nitrogen fixation |
| CN114538817A (en) * | 2022-03-24 | 2022-05-27 | 武汉三源特种建材有限责任公司 | Phase-change expansion crack resistance agent for concrete and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586160A (en) * | 2019-09-20 | 2019-12-20 | 济南大学 | Preparation method of cage-shaped cobalt sulfide/graphite phase carbon nitride composite photocatalyst |
| CN111250042A (en) * | 2020-02-18 | 2020-06-09 | 上海电力大学 | Carbon-based adsorbent for demercuration and preparation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586160A (en) * | 2019-09-20 | 2019-12-20 | 济南大学 | Preparation method of cage-shaped cobalt sulfide/graphite phase carbon nitride composite photocatalyst |
| CN111250042A (en) * | 2020-02-18 | 2020-06-09 | 上海电力大学 | Carbon-based adsorbent for demercuration and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113086955A (en) * | 2021-03-30 | 2021-07-09 | 武汉大学 | Preparation method of carbon-deficient carbon nitride material for photocatalytic nitrogen fixation |
| CN114538817A (en) * | 2022-03-24 | 2022-05-27 | 武汉三源特种建材有限责任公司 | Phase-change expansion crack resistance agent for concrete and preparation method thereof |
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Application publication date: 20201027 |