CN104998674A - Silicate clay-carbon nitride composite material of multilevel structure and preparation method of silicate clay-carbon nitride composite material - Google Patents
Silicate clay-carbon nitride composite material of multilevel structure and preparation method of silicate clay-carbon nitride composite material Download PDFInfo
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- CN104998674A CN104998674A CN201510341186.1A CN201510341186A CN104998674A CN 104998674 A CN104998674 A CN 104998674A CN 201510341186 A CN201510341186 A CN 201510341186A CN 104998674 A CN104998674 A CN 104998674A
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Abstract
The invention belongs to the field of inorganic nonmetal matrix composite materials, and discloses a silicate clay-carbon nitride composite material of a multilevel structure. Silicate clay is adopted as a kernel body, and the surface of the silicate clay is loaded with carbon nitride to form a carbon nitride nanosheet of the multilevel structure A preparation method comprises the following steps that 1, the silicate clay is evenly dispersed in a formaldehyde solution, the system pH value is adjusted while stirring, then melamine is added to obtain mixed dispersion liquid, stirring continues to be carried out for a heat preservation reaction, the acidity of the system pH value is adjusted with an acid solution, a consistent-temperature reaction continues, the system pH value is adjusted with an alkaline solution, and complex liquid is prepared; 2, the complex liquid is dried, then a pyrolytic reaction is carried out under nitrogen atmosphere, and the silicate clay-carbon nitride composite material is prepared. Carbon and nitrogen in resin can be nucleated in the silicate clay, and grow in situ to the carbon nanosheet of the multilevel structure, and therefore agglomeration or folding of the carbon nitride nanosheet is avoided effectively, and the specific surface area of the composite material is improved.
Description
Technical field
The invention belongs to inorganic non-metallic based composites field, be specifically related to a kind of preparation method with the silicate clay/carbonitride composite of multilevel hierarchy.
Background technology
Graphite phase carbon nitride (g-C
3n
4) be a kind ofly novel there is visible light-responded non-metal optical catalysis material, be used to photodissociation aquatic products hydrogen because of advantages such as the semiconductor energy band structure of its uniqueness and excellent chemical stabilities and produce the fields such as oxygen, the organic selectivity synthesis of photocatalysis, photocatalysis degradation organic contaminant.But, g-C
3n
4exist specific area less, in water the shortcoming such as bad dispersibility, thus constrain its photocatalysis performance.For this reason usually through change g-C
3n
4microstructure, as design loose structure, preparation nanometer rods and nano thin-layer etc. solve this problem, but still there is certain defect in said method.Synthesizing porous g-C
3n
4, then need to add template and remove the operations such as template again and come, and prepare g-C
3n
4nano thin-layer often adopts solvent stripping method; These methods all make g-C
3n
4production technology relative complex, time consumption and energy consumption, cost increases.Chinese patent CN 103539090B has synthesized the azotized carbon nano rod array of the uniform high orientations of a kind of appearance and size, but the method through high-temperature water thermal technology sequence, need be not suitable for large-scale production.Therefore, how adopting a kind of relatively simple method to prepare the carbon nitride material having high-ratio surface sum superior dispersibility energy concurrently is the key technical problem that will solve.
Summary of the invention
The present invention overcomes the deficiency of graphite-phase silicon nitride complicated process of preparation in prior art; silicate clay-carbonitride composite that a kind of multilevel hierarchy is provided and preparation method thereof; the method has the features such as simple, with low cost; be applicable to large-scale production, this carbonitride composite has high-ratio surface sum superior dispersibility energy concurrently.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is, silicate clay-carbonitride composite of multilevel hierarchy, with the silicate clay of one-dimensional nano structure for nucleome, carbonitride load forms the azotized carbon nano sheet of multilevel hierarchy at silicate clay surfaces.
As preferably, described silicate clay is the one in attapulgite, galapectite or sepiolite.
The preparation method of above-mentioned silicate clay-carbonitride composite, step is as follows:
(1) evenly spread in formalin by silicate clay, stirring lower adjustment system pH is 8.5 ~ 10.0, and then adding melamine obtains mixed dispersion liquid, system is warming up to 80 ~ 90 DEG C, continues to stir insulation reaction 30 ~ 60 minutes; Be 4.0 ~ 5.8 by acid solution regulation system pH value, continue isothermal reaction, when mixed liquor instillation deionization with in present white vaporific and not easily scatter time, be 7.5 ~ 9.0 with alkaline solution regulation system pH value immediately, obtain silicate clay/melamine formaldehyde resin complex liquid;
(2) silicate clay/melamine formaldehyde resin complex liquid that step (1) is obtained is dried under temperature is 80 DEG C ~ 100 DEG C conditions, then being placed in temperature is in a nitrogen atmosphere carry out pyrolytic reaction 4 ~ 10 hours under 450 DEG C ~ 650 DEG C conditions, i.e. obtained silicate clay/carbonitride composite.
As preferably, described formalin mass percentage concentration is 37% ~ 40%.
As preferably, described formaldehyde and melamine mass ratio are 0.30 ~ 1:1, and the formaldehyde in silicate clay quality and mixed liquor and melamine gross mass ratio are 0.1 ~ 0.3:1.
Further, described alkaline solution is the one in sodium hydroxide solution, potassium hydroxide solution or ammonia spirit, and the mass percentage concentration of alkaline solution is 10% ~ 25%.
Further, described acid solution is the one in formic acid solution, acetic acid solution or ammonium chloride solution, and the mass percentage concentration of acid solution is 5 ~ 15%.
Beneficial effect of the present invention:
1, the present invention with the silicate clay of one-dimensional nano structure for nucleome, by " in-situ polymerization-pyrolysis " method namely first at silicate clay surfaces in-situ polymerization melamine formaldehyde resin, then pyrolytic reaction is passed through, prepare silicate clay/carbonitride composite, it is advantageous that: " skeleton " effect taking full advantage of the silicate clay of one-dimensional nano structure, carbon in resin, nitrogen element can at its surface nucleation, growth in situ becomes to have the azotized carbon nano sheet of multilevel hierarchy, thus effectively prevent the reunion of azotized carbon nano sheet and fold, improve the specific area of composite.
2, in the pyrolytic reaction process preparing silicate clay/carbonitride composite, lattice ion (as Fe, Mn etc.) in silicate clay mineral can carry out Effective Doping to carbonitride, thus the band gap of carbon nitride material can be reduced, improve its photocatalysis performance.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) photo of the attapulgite/carbonitride composite by embodiment 5 preparation.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but invention which is intended to be protected is not limited to the scope involved by embodiment:
Embodiment 1
1, it is in the formalin of 37% that 2.4 kilograms of attapulgites are evenly spread to 5.0 kilogram-mass percentage concentrations, stir while use mass percentage concentration be 10% sodium hydroxide solution regulation system pH value be 8.5, then add 6.2 kilograms of melamines and obtain mixed dispersion liquid, system is warming up to 80 DEG C, continue to stir insulation reaction 60 minutes, be 5.8 by the formic acid solution regulation system pH value that mass percentage concentration is 5%, continue isothermal reaction, when presenting white in mixed liquor instillation deionized water and be vaporific and not easily scattering, be 7.5 by the sodium hydroxide solution regulation system pH value that mass percentage concentration is 10% immediately, obtained attapulgite/melamine formaldehyde resin complex liquid,
2, the attapulgite obtained by step 1/melamine formaldehyde resin complex liquid is dried under temperature is 100 DEG C of conditions, then in a nitrogen atmosphere, being placed in temperature is carry out pyrolytic reaction 10 hours under 450 DEG C of conditions, i.e. obtained attapulgite/carbonitride composite.
Embodiment 2
1, it is in the formalin of 40% that 1.2 kilograms of galapectites are evenly spread to 15.0 kilogram-mass percentage concentrations, stir while use mass percentage concentration be 25% potassium hydroxide solution regulation system pH value be 10.0, then add 6.0 kilograms of melamines and obtain mixed dispersion liquid, system is warming up to 90 DEG C, continue to stir insulation reaction 30 minutes, be 4.0 by the ammonium chloride solution regulation system pH value that mass percentage concentration is 15%, continue isothermal reaction, when presenting white in mixed liquor instillation deionized water and be vaporific and not easily scattering, be 9.0 by the potassium hydroxide solution regulation system pH value that mass percentage concentration is 25% immediately, obtained galapectite/melamine formaldehyde resin complex liquid,
2, dried under temperature is 80 DEG C of conditions by the galapectite obtained by step 1/melamine formaldehyde resin complex liquid, then in a nitrogen atmosphere, being placed in temperature is carry out pyrolytic reaction 4 hours under 650 DEG C of conditions, i.e. obtained galapectite/carbonitride composite.
Embodiment 3
1, it is in the formalin of 38% that 1.5 kilograms of sepiolites are evenly spread to 7.5 kilogram-mass percentage concentrations, stir while use mass percentage concentration be 17.5% ammonia spirit regulation system pH value be 9.5, then add 4.8 kilograms of melamines and obtain mixed dispersion liquid, system is warming up to 85 DEG C, continue to stir insulation reaction 45 minutes, be 5.0 by the acetic acid solution regulation system pH value that mass percentage concentration is 10%, continue isothermal reaction, when presenting white in mixed liquor instillation deionized water and be vaporific and not easily scattering, be 8.5 by the ammonia spirit regulation system pH value that mass percentage concentration is 17.5% immediately, obtained sepiolite/melamine formaldehyde resin complex liquid,
2, dried under temperature is 90 DEG C of conditions by the sepiolite obtained by step 1/melamine formaldehyde resin complex liquid, then in a nitrogen atmosphere, being placed in temperature is carry out pyrolytic reaction 7 hours under 550 DEG C of conditions, i.e. obtained sepiolite/carbonitride composite.
Embodiment 4
1, it is in the formalin of 39% that 0.95 kilogram of galapectite is evenly spread to 5.0 kilogram-mass percentage concentrations, stir while use mass percentage concentration be 15% potassium hydroxide solution regulation system pH value be 9.0, then add 4.3 kilograms of melamines and obtain mixed dispersion liquid, system is warming up to 83 DEG C, continue to stir insulation reaction 50 minutes, be 4.5 by the acetic acid solution regulation system pH value that mass percentage concentration is 10%, continue isothermal reaction, when presenting white in mixed liquor instillation deionized water and be vaporific and not easily scattering, be 8.0 by the potassium hydroxide solution regulation system pH value that mass percentage concentration is 15% immediately, obtained galapectite/melamine formaldehyde resin complex liquid,
2, dried under temperature is 95 DEG C of conditions by the galapectite obtained by step 1/melamine formaldehyde resin complex liquid, then in a nitrogen atmosphere, being placed in temperature is carry out pyrolytic reaction 8 hours under 500 DEG C of conditions, i.e. obtained galapectite/carbonitride composite.
Embodiment 5
1, it is in the formalin of 37% that 1.0 kilograms of attapulgites are evenly spread to 5.0 kilogram-mass percentage concentrations, stir while use mass percentage concentration be 10% sodium hydroxide solution regulation system pH value be 9.5, then add 2.2 kilograms of melamines and obtain mixed dispersion liquid, system is warming up to 85 DEG C, continue to stir insulation reaction 55 minutes, be 4.8 by the formic acid solution regulation system pH value that mass percentage concentration is 5%, continue isothermal reaction, when presenting white in mixed liquor instillation deionized water and be vaporific and not easily scattering, be 8.5 by the sodium hydroxide solution regulation system pH value that mass percentage concentration is 10% immediately, obtained attapulgite/melamine formaldehyde resin complex liquid,
2, the attapulgite obtained by step 1/melamine formaldehyde resin complex liquid is dried under temperature is 85 DEG C of conditions, then in a nitrogen atmosphere, being placed in temperature is carry out pyrolytic reaction 6 hours under 600 DEG C of conditions, i.e. obtained attapulgite/carbonitride composite.As can be seen from Figure 1, there is the growth of laminar structured, that particle size is about 50nm carbonitride on the brilliant surface of attapulgite rod, thus define the attapulgite/carbonitride composite with multilevel hierarchy.
Comparative example 1
Embodiment 5 is compared, its technology operation for first to prepare melamine formaldehyde resin, and with attapulgite physical mixed after carry out pyrolytic reaction again, obtained attapulgite/carbonitride composite, concrete operation step is as follows:
1, while stir, while be drip the sodium hydroxide solution that mass percentage concentration is 10% in the formalin of 37% to 5.0 kilogram-mass percentage concentrations, regulation system pH value is 9.5, then add 2.2 kilograms of melamines and obtain mixed dispersion liquid, system is warming up to 85 DEG C, continue to stir insulation reaction 55 minutes, be 4.8 by the formic acid solution regulation system pH value that mass percentage concentration is 5%, continue isothermal reaction, when presenting white in mixed liquor instillation deionized water and be vaporific and not easily scattering, be 8.5 by the sodium hydroxide solution regulation system pH value that mass percentage concentration is 10% immediately, obtained melamine formaldehyde resin,
2, by the melamine formaldehyde resin mixing obtained by 1 kilogram of attapulgite and step 1, and in a nitrogen atmosphere, being placed in temperature is carry out pyrolytic reaction 6 hours under 600 DEG C of conditions, i.e. obtained attapulgite/carbonitride composite.80.0m can be reached by the composite specific area obtained by embodiment 5
2/ g, the composite specific area obtained by comparative example 1 can reach 41.6m
2/ g.
Claims (7)
1. silicate clay-carbonitride composite of multilevel hierarchy, is characterized in that: with the silicate clay of one-dimensional nano structure for nucleome, and carbonitride load forms the azotized carbon nano sheet of multilevel hierarchy at silicate clay surfaces.
2. silicate clay-carbonitride the composite of multilevel hierarchy according to claim 1, is characterized in that: described silicate clay is the one in attapulgite, galapectite or sepiolite.
3. the preparation method of silicate clay according to claim 1 and 2-carbonitride composite, it is characterized in that, step is as follows:
(1) evenly spread in formalin by silicate clay, stirring lower adjustment system pH is 8.5 ~ 10.0, and then adding melamine obtains mixed dispersion liquid, system is warming up to 80 ~ 90 DEG C, continues to stir insulation reaction 30 ~ 60 minutes; Be 4.0 ~ 5.8 by acid solution regulation system pH value, continue isothermal reaction, when mixed liquor instillation deionization with in present white vaporific and not easily scatter time, be 7.5 ~ 9.0 with alkaline solution regulation system pH value immediately, obtain silicate clay/melamine formaldehyde resin complex liquid;
(2) silicate clay/melamine formaldehyde resin complex liquid that step (1) is obtained is dried under temperature is 80 DEG C ~ 100 DEG C conditions, then being placed in temperature is in a nitrogen atmosphere carry out pyrolytic reaction 4 ~ 10 hours under 450 DEG C ~ 650 DEG C conditions, i.e. obtained silicate clay/carbonitride composite.
4. the preparation method of silicate clay according to claim 3-carbonitride composite, is characterized in that: described formalin mass percentage concentration is 37% ~ 40%.
5. the preparation method of silicate clay according to claim 3-carbonitride composite, it is characterized in that: described formaldehyde and melamine mass ratio are 0.30 ~ 1:1, the formaldehyde in silicate clay quality and mixed liquor and melamine gross mass ratio are 0.1 ~ 0.3:1.
6. the preparation method of silicate clay according to claim 3-carbonitride composite, it is characterized in that: described alkaline solution is the one in sodium hydroxide solution, potassium hydroxide solution or ammonia spirit, the mass percentage concentration of alkaline solution is 10% ~ 25%.
7. the preparation method of silicate clay according to claim 3-carbonitride composite, is characterized in that: described acid solution is the one in formic acid solution, acetic acid solution or ammonium chloride solution, and the mass percentage concentration of acid solution is 5 ~ 15%.
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| CN106040278A (en) * | 2016-06-12 | 2016-10-26 | 湘潭大学 | Preparation method and application of Pd-Ni bimetallic catalyst supported by N-doped acid-activated sepiolite |
| CN106117604A (en) * | 2016-07-15 | 2016-11-16 | 江苏省华源矿业有限公司 | The preparation method of absorbent-type attapulgite ground mass fire proofing |
| CN107088397A (en) * | 2017-05-02 | 2017-08-25 | 常州大学 | A kind of silicate clay/small size nitridation carbon composite and preparation method thereof |
| CN107185575A (en) * | 2017-05-23 | 2017-09-22 | 江苏大学 | A kind of mesoporous g C of binary intercalation3N4The Preparation method and use of@ATP composite photo-catalysts |
| 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 |
| CN108147380A (en) * | 2018-01-08 | 2018-06-12 | 湘潭大学 | A kind of preparation method of honeycomb carbonitride |
| CN108816268A (en) * | 2018-07-04 | 2018-11-16 | 西南科技大学 | Composite photocatalyst nano material and preparation method thereof and degradation of contaminant method |
| CN109482873A (en) * | 2018-12-30 | 2019-03-19 | 镇江汇通金属成型有限公司 | A kind of preparation method of the copper mould for turbine casting |
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| CN105396605A (en) * | 2015-11-09 | 2016-03-16 | 常州大学 | Preparation method of silicate clay/copper/carbon nitride composite material |
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| US20220305475A1 (en) * | 2020-05-27 | 2022-09-29 | Changzhou University | Method for preparing silicate/carbon composite from attapulgite, and use of silicate/carbon composite |
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