CN117865116A - Preparation method of nitrogen-doped porous carbon material with one-dimensional and two-dimensional structure - Google Patents
Preparation method of nitrogen-doped porous carbon material with one-dimensional and two-dimensional structure Download PDFInfo
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 41
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000003960 organic solvent Substances 0.000 claims abstract description 16
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 14
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 14
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 25
- 238000001179 sorption measurement Methods 0.000 claims description 21
- 239000003463 adsorbent Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 17
- 229910052799 carbon Inorganic materials 0.000 abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 13
- 230000034655 secondary growth Effects 0.000 abstract description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 20
- 239000000463 material Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 description 4
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
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- VYQRBKCKQCRYEE-UHFFFAOYSA-N ctk1a7239 Chemical compound C12=CC=CC=C2N2CC=CC3=NC=CC1=C32 VYQRBKCKQCRYEE-UHFFFAOYSA-N 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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Abstract
The application discloses a preparation method of a nitrogen-doped porous carbon material with a one-dimensional and two-dimensional structure, which comprises the following steps: s1, carrying out hydrothermal reaction on a raw material liquid containing zinc nitrate, benzimidazole, hexamethylenetetramine and a solvent to obtain MOFs raw material; s2, ball milling the MOFs raw material obtained in the step S1 in a mixed solution of an organic solvent and water to obtain the MOFs raw material with a one-dimensional and two-dimensional structure; and S3, calcining the MOFs raw material with the one-dimensional and two-dimensional structure obtained in the step S2 in an inactive atmosphere to obtain the nitrogen-doped porous carbon material with the one-dimensional and two-dimensional structure. The method is simple in preparation, and the nitrogen doped porous carbon with a one-dimensional and two-dimensional structure can be formed by using different solvents and not needing secondary growth only through ball milling.
Description
Technical Field
The application relates to a preparation method of a nitrogen-doped porous carbon material with a one-dimensional and two-dimensional structure, and belongs to the technical field of new material preparation.
Background
Sulfur dioxide (SO) 2 ) Is one of the main pollutants causing the atmospheric pollution, is the main cause of the air quality deterioration and the increasingly serious hazard of acid rain, so sulfur dioxide is one of the atmospheric pollutants with the total amount controlled specified in China. Currently, the method is thatThe most widely used desulfurization technique is wet desulfurization, but the method can produce a large amount of wastewater and industrial byproducts, which have a great influence on the environment. In recent years, various types of adsorbents, such as porous carbon, porous organic polymers, metal organic frameworks, and the like, are being widely studied and excellent in performance, and exhibit good application prospects. The porous carbon-based material is a material with a porous structure taking carbon elements as a matrix, has the advantages of wide sources, low cost, rich types, high thermal stability, strong chemical reaction inertia, larger specific surface area, rich pore channel structures, easy regulation and control of the pore channel surface environment and the like, and has certain advantages in the adsorption field. However, the adsorption capacity of pure carbon materials is still difficult to meet current requirements. The adsorption performance of the porous carbon-based material is not only related to the pore channel structure, but also has a key effect on the surface chemical environment of the pore channel. A great deal of researches prove that the increase of the alkaline environment on the surface of the porous carbon pore canal can promote the adsorption of acid gas, thereby improving the corresponding selective adsorption capacity. Taking into account SO 2 The acidic nature of the carbon material may be modified by nitrogen doping. When the surface of the carbon material contains basic functional groups containing nitrogen, SO is generated due to the interaction of acid and alkali 2 The molecules may be more efficiently adsorbed. More importantly, the nitrogen doping changes the surface electrostatic potential of adjacent carbon atoms, and increases the local electron density, the polarity of the carbon atoms and the surface charge distribution of the adjacent carbon atoms through the conjugation effect, thereby enhancing SO 2 Interaction of molecules with the carbon surface. Among these, the nitrogen-doped carbon nanowires and carbon nanoplates have excellent physicochemical properties due to unique one-dimensional linear and two-dimensional planar structures, and are effectively utilized in the adsorption field. The two are compounded, a hierarchical pore structure can be constructed by utilizing the synergistic effect of carbon materials with different dimensions, and SO is enhanced 2 Is a component of the adsorption process. However, the current one-dimensional and two-dimensional material compounding method is either a simple physical mixing method or a one-dimensional carbon material growth method by taking a two-dimensional material as a substrate. Simple physical mixing affects the interaction of two-dimensional materials of one-dimensional materials, whereas regrowth based on two-dimensional carbon materials generally requires higher temperatures and metal catalystsThe energy consumption is high, and the metal catalyst used needs to be further removed, so that the complexity of the steps is increased. In addition, an external nitrogen source is selected in the nitrogen doping process, but the external unit is difficult to realize uniform distribution of nitrogen elements, and the structural collapse of the carbon material is easy to cause, so that the shape is not easy to maintain. Therefore, development of a new preparation method of nitrogen-doped porous carbon material with one-dimensional and two-dimensional structure and application of the material in SO is needed 2 In adsorption.
Disclosure of Invention
According to one aspect of the application, the preparation method of the nitrogen-doped porous carbon material with the one-dimensional and two-dimensional structure is simple and reliable, the prepared material has good adsorption performance, and the problems that the interaction of the one-dimensional material and the two-dimensional material is influenced by simple physical mixing, the regrowth method based on the two-dimensional carbon material is high in energy consumption and complicated in steps, the uniform distribution of nitrogen elements is difficult to realize due to the additional nitrogen source, and the collapse of the structure of the carbon material is easy to cause are solved.
The application adopts the following technical scheme:
a preparation method of a nitrogen-doped porous carbon material with a one-dimensional and two-dimensional structure comprises the following steps:
s1, carrying out hydrothermal reaction on a raw material liquid containing zinc nitrate, benzimidazole, hexamethylenetetramine and a solvent to obtain MOFs raw material;
s2, ball milling the MOFs raw material obtained in the step S1 in a mixed solution of an organic solvent and water to obtain the MOFs raw material with a one-dimensional and two-dimensional structure;
and S3, calcining the MOFs raw material with the one-dimensional and two-dimensional structure obtained in the step S2 in an inactive atmosphere to obtain the nitrogen-doped porous carbon material with the one-dimensional and two-dimensional structure.
Optionally, in the step S1, the molar ratio of the mixture of benzimidazole and hexamethylenetetramine to zinc nitrate is 1:1-5.
Optionally, in the step S1, the molar ratio of the mixture of benzimidazole and hexamethylenetetramine to zinc nitrate is 1:2-3.
Optionally, the molar ratio of the benzimidazole to the hexamethylenetetramine is 4-9:1.
The addition of hexamethylenetetramine in the present application can regulate the structure of the resulting MOFs so that they have thinner and more uniform lamellae.
Optionally, in step S1, the solvent is selected from N, N-dimethylformamide.
Optionally, in step S1, the solid-to-liquid ratio of zinc nitrate to solvent is 10-50 mmol/1L.
Optionally, in step S1, the hydrothermal reaction conditions include: the reaction temperature is 70-130 ℃ and the reaction time is 20-50 h.
Optionally, in step S1, the product is washed with absolute ethanol and dried at room temperature after the hydrothermal reaction.
Optionally, in step S2, the organic solvent is selected from N, N-dimethylformamide.
Optionally, in the step S2, the solid-to-liquid ratio of MOFs raw material to the mixed solution of the organic solvent and water is 10-50 mg/1 mL;
optionally, in the mixed solution of the organic solvent and the water, the volume ratio of the organic solvent to the water is 1-9:1.
Optionally, the volume ratio of the organic solvent to the water in the mixed solution of the organic solvent and the water is selected from any value in 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, or a range value between any two.
Optionally, in the mixed solution of the organic solvent and the water, the volume ratio of the organic solvent to the water is 4-2.35:1;
optionally, the ball milling conditions include: the rotation speed is 100-200 rpm.
In the application, in step S2, the difference of specific heat capacities of the organic solvent and water (for example, DMF specific heat capacity is 2140kJ/kg ℃ and water specific heat capacity is 4200kJ/kg ℃) is utilized, so that heat difference force is generated by instantaneous temperature rise of the MOFs sheet layer in the ball milling process, and part of the sheet layer is promoted to curl to form one-dimensional nanowires, so that MOFs with one-dimensional and two-dimensional structures are formed.
Optionally, in step S3, the calcining conditions include: the temperature rising speed is 3-10 ℃/min, the calcining temperature is 700-1000 ℃ and the calcining time is 1-3 h.
According to another aspect of the application, the nitrogen-doped porous carbon material with a one-dimensional and two-dimensional structure, which is prepared by the preparation method, is also provided.
According to another aspect of the present application, there is also provided a method for preparing the nitrogen-doped porous carbon material with one-dimensional and two-dimensional structure as an adsorbent in SO 2 Application in adsorption.
The beneficial effects that this application can produce include:
the preparation method of the nitrogen-doped porous carbon material with the one-dimensional and two-dimensional structure has the following beneficial effects: 1) The preparation method is simple, and the nitrogen doped porous carbon with a one-dimensional and two-dimensional structure can be formed by using different solvents without secondary growth through ball milling; 2) The porous carbon with one-dimensional and two-dimensional structure can provide a hierarchical pore structure, which is more beneficial to SO 2 Is transported and adsorbed; 3) The nitrogen element of MOFs framework can ensure that the prepared porous carbon has higher nitrogen content which can reach 9.2 weight percent, and metal zinc can form micropores through sublimation in the carbonization process, SO that SO is promoted 2 Is used for the adsorption capacity of the catalyst; 4) The addition of hexamethylenetetramine in the coordination process can thin the sheet layer, which is beneficial to the change of the structure in the ball milling process; 5) The porous carbon prepared at 25 ℃ can absorb 96mg of SO at the maximum per gram under normal pressure 2 。
Drawings
FIG. 1 is an SEM image of example 2 of the present application, with dimensions of 1 μm.
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
Unless otherwise indicated, all starting materials in the examples of the present application were purchased commercially.
In the application, the nitrogen-doped porous carbon material SO with one-dimensional and two-dimensional structure 2 The adsorption conditions for the adsorption experiments were as follows: the total feed gas was 1200ppm SO 2 And balance gas N 2 The flow rate was 30mL/min, the adsorption temperature was 25℃and the adsorbent amount was 50mg.
Example 1
1) Preparation of layered MOFs
1mmol of zinc nitrate hexahydrate, 0.9mmol of benzimidazole and 0.1mmol of hexamethylenetetramine are dispersed into DMF solution, stirred and dissolved, placed into a hydrothermal kettle and reacted for 50 hours at 70 ℃. Washing with absolute ethanol, and drying at room temperature
2) Ball milling layered MOFs
2.1 100mg of layered MOFs sample is placed in a 50mL ball milling tank, 10mL of DMF/water solution (9:1) is added, and ball milling is performed for 2 hours at a rotating speed of 100 revolutions per minute to obtain MOFs with one-dimensional and two-dimensional structures.
3) Preparation of nitrogen-doped hollow carbon sphere/MOF-based porous carbon composite material
And (3) placing 100mg MOFs sample into a tube furnace, heating to 700 ℃ at a speed of 3 ℃/min under the protection of inert gas, carbonizing for 3 hours, and cooling to room temperature to obtain the nitrogen-doped porous carbon material with the one-dimensional and two-dimensional structure.
Through SO 2 Adsorption experiments show that the adsorption capacity of the adsorbent can reach 82mg/.
Example 2
1) Preparation of layered MOFs
2mmol of zinc nitrate hexahydrate, 0.8mmol of benzimidazole and 0.2mmol of hexamethylenetetramine are dispersed into DMF solution, stirred and dissolved, placed into a hydrothermal kettle and reacted for 40 hours at the temperature of 100 ℃. Washing with absolute ethanol, and drying at room temperature
2) Ball milling layered MOFs
2.1 300mg of layered MOFs sample is placed in a 50mL ball milling tank, 10mL of DMF/water solution (7:3) is added, and ball milling is performed for 4 hours at a rotating speed of 150 revolutions per minute to obtain MOFs with one-dimensional and two-dimensional structures.
3) Preparation of nitrogen-doped hollow carbon sphere/MOF-based porous carbon composite material
And (3) placing 100mg MOFs sample into a tube furnace, heating to 900 ℃ at a speed of 5 ℃/min under the protection of inert gas, carbonizing for 2 hours, and cooling to room temperature to obtain the nitrogen-doped porous carbon material with one-dimensional and two-dimensional structure (the microscopic morphology is shown in figure 1). The nitrogen content of the resulting material may reach 9.2wt%.
Through SO 2 Adsorption experiments show that the adsorption capacity of the adsorbent can reach 96mg/g.
Example 3
1) Preparation of layered MOFs
5mmol of zinc nitrate hexahydrate, 0.8mmol of benzimidazole and 0.2mmol of hexamethylenetetramine are dispersed into DMF solution, stirred and dissolved, placed into a hydrothermal kettle and reacted for 24 hours at 130 ℃. Washing with absolute ethanol, and drying at room temperature
2) Ball milling layered MOFs
2.1 500mg of layered MOFs sample is placed in a 50mL ball milling tank, 10mL of DMF/water solution (1:1) is added, and ball milling is performed for 5 hours at a rotating speed of 200 revolutions per minute to obtain MOFs with one-dimensional and two-dimensional structures.
3) Preparation of nitrogen-doped hollow carbon sphere/MOF-based porous carbon composite material
And (3) placing 100mg MOFs sample into a tube furnace, heating to 1000 ℃ at a speed of 10 ℃/min under the protection of inert gas, carbonizing for 1h, and cooling to room temperature to obtain the nitrogen-doped porous carbon material with one-dimensional and two-dimensional structures.
Through SO 2 Adsorption experiments show that the adsorption capacity of the adsorbent can reach 90mg/g.
Comparative example 1
1) Preparation of layered MOFs
1mmol of zinc nitrate hexahydrate, 0.9mmol of benzimidazole and 0.1mmol of hexamethylenetetramine are dispersed into DMF solution, stirred and dissolved, placed into a hydrothermal kettle and reacted for 50 hours at 70 ℃. Washing with absolute ethanol, and drying at room temperature
2) Ball milling layered MOFs
2.1 100mg of layered MOFs sample is placed in a 50mL ball milling tank, 10mL of aqueous solution is added, and the MOFs with one-dimensional and two-dimensional structures cannot be obtained after ball milling for 2 hours at the rotating speed of 100 rpm.
The foregoing description is only a few examples of the present application and is not intended to limit the present application in any way, and although the present application is disclosed in the preferred examples, it is not intended to limit the present application, and any person skilled in the art may make some changes or modifications to the disclosed technology without departing from the scope of the technical solution of the present application, and the technical solution is equivalent to the equivalent embodiments.
Claims (10)
1. The preparation method of the nitrogen-doped porous carbon material with the one-dimensional and two-dimensional structure is characterized by comprising the following steps of:
s1, carrying out hydrothermal reaction on a raw material liquid containing zinc nitrate, benzimidazole, hexamethylenetetramine and a solvent to obtain MOFs raw material;
s2, ball milling the MOFs raw material obtained in the step S1 in a mixed solution of an organic solvent and water to obtain the MOFs raw material with a one-dimensional and two-dimensional structure;
and S3, calcining the MOFs raw material with the one-dimensional and two-dimensional structure obtained in the step S2 in an inactive atmosphere to obtain the nitrogen-doped porous carbon material with the one-dimensional and two-dimensional structure.
2. The method according to claim 1, wherein in the step S1, the molar ratio of the mixture of benzimidazole and hexamethylenetetramine to zinc nitrate is 1:1-5.
3. The method according to claim 1, wherein in the step S1, the molar ratio of benzimidazole to hexamethylenetetramine is 4-9:1.
4. The method according to claim 1, wherein in step S1, the solid-to-liquid ratio of zinc nitrate to the solvent is 10 to 50 mmol/1L.
5. The method according to claim 1, wherein in step S1, the hydrothermal reaction conditions include: the reaction temperature is 70-130 ℃ and the reaction time is 20-50 h.
6. The method according to claim 1, wherein in step S2, the organic solvent is selected from the group consisting of N, N-dimethylformamide.
7. The method according to claim 1, wherein in step S2, the solid-to-liquid ratio of MOFs raw material to the mixture of organic solvent and water is 10-50 mg/1 mL;
preferably, in the mixed solution of the organic solvent and the water, the volume ratio of the organic solvent to the water is 1-9:1;
preferably, the ball milling conditions include: the rotation speed is 100-200 rpm.
8. The method according to claim 1, wherein in step S3, the conditions of the calcination include: the temperature rising speed is 3-10 ℃/min, the calcining temperature is 700-1000 ℃ and the calcining time is 1-3 h.
9. The nitrogen-doped porous carbon material with one-dimensional and two-dimensional structures prepared by the preparation method according to any one of the claims 1 to 8.
10. The nitrogen-doped porous carbon material with one-dimensional and two-dimensional structure as claimed in claim 9 as an adsorbent in SO 2 Application in adsorption.
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