CN104801326A - Surface-hydroxylated nano-pore carbon nitride photocatalytic material as well as preparation method and application thereof - Google Patents
Surface-hydroxylated nano-pore carbon nitride photocatalytic material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a surface-hydroxylated nano-pore carbon nitride photocatalytic material as well as a preparation method and an application thereof. A nano-pore structure of the photocatalytic material mainly comprises mesopores with diameters of 5-30 nm and comprises micropores with diameters smaller than 2 nm, the specific surface area is 10-90 m<2>/g, and a hydroxyl group is grafted on the surface; during preparation, melamine, alkali chloride and alkali containing alkali metal or alkaline-earth metal elements are taken as raw materials and treated in an electric furnace at the temperature of 400 DEG C-600 DEG C for certain time, a product is subjected to washing, extraction filtration and separation, the yellow nano-pore carbon nitride photocatalytic material is obtained, and the alkali chloride in a washing solution is recovered. With adoption of the method, a little alkali is taken as a pore forming material, meanwhile, a catalyst forms a hydroxylation surface, no template agent and surfactant are required, the cost is reduced, the problems of complicated preparation process, non-environmental protection and low probability of industrialization promotion in the prior art are solved, and the product has excellent capability of photocatalytic degradation on gas-phase pollutants.
Description
Technical field
The present invention relates to a kind of receiving bore catalysis material and its preparation method and application, under particularly relating to a kind of alkali condition, prepare that crystallinity is good, the method for the receiving bore carbonitride catalysis material of surface hydroxylation and the application in degraded vapor phase contaminants.
Background technology
The fast development of modern industry, the living standard of the people is had huge raising, make the mankind in the face of environmental crisis and energy crisis etc., photocatalysis is as an emerging research field, and its technology is expected to solve problem of environmental pollution and energy shortage problem simultaneously simultaneously.Polymer semiconductor's carbonitride, because it is cheap, stable, not the visible-light photocatalysis material of metallic components be widely used in the photocatalytic conversion of solar energy, as photocatalytic water, the degraded of liquid phase organic pollutant, CO
2photo-reduction aspect, has good effect, but also little to the report of gas phase organic pollutant degraded, and degrading activity is poor.
For degrading gaseous-phase organic pollutant, specific area affects the important parameter of of its activity, the receiving bore material of high-specific surface area owing to having more avtive spot, good absorbing properties and there is better activity.In addition, the crystallinity of material is also improve a key factor of photocatalytic activity, and therefore the nano pore structure of material and good crystalline combination may obtain active more excellent carbon nitride material.This research has great importance for obtaining the material with excellent visible light photocatalysis active.
Nitride porous carbon mainly refers to mesoporous carbonitride, and the main method preparing mesoporous carbonitride is hard template method, as the people such as Wang Xinchen report at J.Am.Chem.Soc. magazine (the 131st phase 1680-1681 page in 2009) with SiO
2nano particle is template, prepared different specific area carbonitride.But this class methods complex process, not environmentally.In the recent period, the people such as Yan Shicheng have developed again a kind of molten-salt growth method to prepare mesoporous carbonitride (patent No. CN 102992282 B), and carbonitride is wrapped in the growth of fused salt droplet, forms mesoporous carbonitride.But mesoporous carbonitride prepared by molten-salt growth method is only applied to photolysis water hydrogen, does not relate to the application of photocatalytic degradation vapor phase contaminants aspect.
Summary of the invention
In order to solve problems of the prior art, receiving bore carbonitride catalysis material that the invention provides a kind of surface hydroxylation and its preparation method and application, solve existing organic catalysis material degrading gaseous-phase organic pollutant degraded performance and complicated process of preparation, not environmentally, not easily realize the difficulties such as Industry Promotion.
Technical scheme of the present invention is:
A kind of surface hydroxylation receiving bore carbonitride catalysis material, the nano pore structure of described catalysis material is the mesoporous of 5 ~ 30nm based on aperture, and is less than the micropore of 2nm containing aperture, and specific area is 10 ~ 90m
2/ g, surface graft has oh group.
A preparation method for surface hydroxylation receiving bore carbonitride catalysis material, with melamine, alkali metal chloride and alkali for raw material, one-step method directly obtains the receiving bore carbonitride of surface hydroxylation.
The preparation method of surface hydroxylation receiving bore carbonitride catalysis material, comprises the steps:
(1) by the grinding of the mixture of melamine, alkali metal chloride and alkali evenly;
(2) mixture in step (1) be placed in crucible and close, in Muffle furnace, 400 ~ 600 DEG C process 2 ~ 4 hours;
(3) product in step (2) is dissolved in deionized water, stirs, suspension filter paper is carried out suction filtration washing, alkali metal chloride in recycle-water washing lotion, product is placed in baking oven dry, then grinds, obtain end product.
In described step (1), alkali metal chloride is reaction promoter, comprises sodium chloride, potassium chloride or lithium chloride.
In described step (1), alkali is the alkali of alkali metal containing or alkali earth metal, is pore creating material and the raw material producing surface hydroxyl, comprises potassium hydroxide, NaOH, lithium hydroxide or strontium hydroxide.
In described step (1), the mass ratio of melamine and chloride salt is in 0.05 ~ 10 scope, and the quality of alkali is 0.5% ~ 3% of the gross mass of melamine and chloride salt.More preferably, the mass ratio of melamine and chloride salt is 0.2.
Described step (2) to be preferably in Muffle furnace 550 DEG C of process 4 hours.
The application of surface hydroxylation receiving bore carbonitride catalysis material in degrading gaseous-phase organic pollutant, described gaseous-phase organic pollutant comprises alcohol, aldehyde, ketone, acid and aromatic compound.
The invention has the beneficial effects as follows: 1. the multifunctionality of alkali in synthetic method.In the inventive method, alkali consumption is few, but can realize the function of three aspects, and one is form nano pore structure as a kind of pore creating material original position, increases the specific area of catalysis material; Two is that building-up process situ removes unstable phase, increases the crystallinity of catalysis material; Three is form hydroxyl on catalysis material surface, strengthens catalysis material reactivity.
2. pore passage structure diversification.The receiving bore carbonitride catalysis material that this method is obtained, be the mesoporous of 5 ~ 30nm except having aperture, also there is the micropore that a certain amount of aperture is less than 2nm, highly beneficial for gaseous-phase organic pollutant degraded, organic pollutant molecule can import catalysis material inside into by mesopore orbit, make full use of the inner ratio surface area of catalysis material, more easily in bond until degradable mineralising after entering micropore canals, realize fast organic pollution being removed from gas phase and thoroughly degraded.
3. the high efficiency of light degradation property.Except the advantage that above-mentioned nano pore structure provides, surface hydroxylation also provides decisive power for efficiency light degraded, and surface hydroxyl can strengthen gaseous-phase organic pollutant absorption, also can may be activated into hydroxyl radical free radical, be beneficial to the mineralising of gaseous-phase organic pollutant.
4. synthesis technique is simple, raw material usefulness is high.The raw material that this method uses is common, without special installation needs, use a small amount of alkali but can realize three large effects, and the larger chloride salt of use amount can carry out recycling, as can be seen here, this method compared with the conventional method, simple, high-efficiency environment friendly.
Disclosed by the invention is the receiving bore carbonitride of surface hydroxylation, all have different from microstructure to chemical constituent from prior art: (1) contrasts pore passage structure, nano pore structure has more microcellular structure (aperture is less than 2nm) than meso-hole structure, can gaseous-phase organic pollutant is strapped in pore passage structure; (2) contrast table surface properties, surface hydroxyl turns to the hydrophily that catalysis material provides reactivity site, regulates surface energy band structure, improves material; (3) contrast chemical constituent, surface graft hydroxyl (OH) makes material have higher oxygen and the content of hydrogen.In vapor phase contaminants light degradation, the receiving bore carbonitride of surface hydroxylation has two large advantages: high specific area provides more avtive spot; Surface hydroxyl can interact with gaseous-phase organic pollutant, and promote light degradation reaction, surface hydroxyl also can may be activated into hydroxyl radical free radical, is beneficial to the mineralising of gaseous-phase organic pollutant.
In sum, the invention relates to the innovation of a kind of surface hydroxylation receiving bore carbonitride catalysis material and preparation method thereof.The carbonitride prepared of this method is existing mesoporously has micropore again, and surface graft has hydroxyl simultaneously, is beneficial to the light degradation of gaseous-phase organic pollutant.This method synthesis technique is simple; do not need to add any template and surfactant; non-template method one step is adopted to prepare receiving bore carbonitride; a kind of simple, environmental friendliness, the preparation method being applicable to the receiving bore carbonitride of industrialization large-scale production; raw material usefulness is high; product has the performance of excellent photocatalytic degradation gaseous-phase organic pollutant, has the great potential promoted to large-scale production.
Accompanying drawing explanation
Fig. 1: X-ray diffraction (XRD) spectrogram of the receiving bore carbonitride of preparation in embodiment 1;
Fig. 2: the nitrogen adsorption-desorption curve of the receiving bore carbonitride of preparation in embodiment 1, illustration is graph of pore diameter distribution;
Fig. 3: ESEM (SEM) photo of the receiving bore carbonitride of preparation in embodiment 1;
Fig. 4: transmission electron microscope (TEM) photo of the receiving bore carbonitride of preparation in embodiment 1.
Concrete embodiment
Also by reference to the accompanying drawings the present invention is further described below by embodiment, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The preparation of surface hydroxylation receiving bore carbonitride: take melamine 1.5g, potassium chloride 7.5g, NaOH 0.1g, mixed-powder grinds 10 ~ 30min in mortar, after fully mixing, be placed in crucible, with aluminium-foil paper, crucible oral area sealed, be placed in Muffle furnace and be warming up to 550 DEG C and be incubated 4h, powder mortar after sintering is levigate, be separated through deionized water suction filtration, dry 4h at 80 DEG C, obtain yellow receiving bore carbonitride.
Some structural researches are carried out to receiving bore carbon nitride product (being labeled as C3N4-KCl/0.1g NaOH) prepared by said method.Fig. 1 is the XRD figure of receiving bore carbon nitride material, illustrates that the product of preparation is carbonitride; BET analysis (Fig. 2) illustrates that carbonitride has and is about 69m
2the specific area of/g, receiving bore size is mainly distributed in about 7nm; Scanning electron microscope (SEM) photograph (Fig. 3) illustrates that the carbonitride particle that product is approximately 70nm by size forms; The nano pore structure that transmission electron microscope (Fig. 4) demonstrates carbonitride further comes from the intergranular hole that size is about 70nm, intergranular hole is approximately about 7nm, and the nano pore of BET graph of pore diameter distribution, TEM figure and SEM figure mutual evidence receiving bore carbonitride comes from the hole between nano particle.It is the carbonitride that melamine (other synthesis conditions are identical, are labeled as C3N4) synthesizes that the photocatalytic degradation gaseous-phase organic pollutant performance of product that as can be seen from Table 1 prepared by the method is far superior to raw material.
Embodiment 2
Sintering temperature and temperature retention time are on the impact of product: the melamine taking 12 parts of 1.5g, the potassium chloride of 7.5g and NaOH 0.1g, mixed-powder grinds 10 ~ 30min in mortar, after fully mixing, be placed in crucible, with aluminium-foil paper, crucible oral area is sealed, be placed in Muffle furnace and be warming up to 400 DEG C respectively, 500 DEG C, 550 DEG C, 600 DEG C, and be incubated 2h respectively at each temperature, 3h, 4h, powder mortar after sintering is levigate, by washed with de-ionized water and suction filtration be separated, separating obtained sample is dry 4h at 80 DEG C, obtain yellow receiving bore carbonitride.Known by the test result comparative analysis of the product to present case, along with the increase of holding temperature rising, temperature retention time, productive rate is more and more lower, and when being incubated 4h at 550 DEG C, productive rate and the quality of the product obtained reach optimal value.
Embodiment 3
Alkali metal chloride consumption is on the impact of product: take the melamine of four parts of 1.5g and the NaOH of 0.1g, potassium chloride 0.15g, 1.5g, 7.5g, 30g is respectively added again in four increment product, raw material is ground 10 ~ 30min in mortar, after fully mixing, be placed in crucible, with aluminium-foil paper, crucible oral area is sealed, be placed in Muffle furnace be warming up to 550 DEG C and be incubated 4h, powder mortar after sintering is levigate, by washed with de-ionized water and suction filtration be separated, separating obtained sample is dry 4h at 80 DEG C, obtains yellow receiving bore carbonitride.Known by the test result analysis of the product to present case, the crystallinity of product and specific area with the increase of alkali metal chloride consumption present first rise after downward trend, when the consumption of potassium chloride is 7.5g, the specific area of product reaches a comparatively figure of merit.
Embodiment 4
Alkali consumption is on the impact of product: take the melamine of four parts of 1.5g and the potassium chloride of 7.5g, NaOH 0.075g, 0.100g, 0.125g, 0.150g is respectively added again in four increment product, raw material is ground 10 ~ 30min in mortar, after fully mixing, be placed in crucible, with aluminium-foil paper, crucible oral area is sealed, be placed in Muffle furnace be warming up to 550 DEG C and be incubated 4h, powder mortar after sintering is levigate, by washed with de-ionized water and suction filtration be separated, separating obtained sample is dry 4h at 80 DEG C, obtains yellow receiving bore carbonitride.Known by the test result analysis of the product to present case, the crystallinity of product and specific area with the increase of alkali consumption present first rise after downward trend, when the consumption of alkali is 0.125g, crystallinity and specific area reach a comparatively figure of merit.
Embodiment 5
Reaction promoter is on the impact of product: take the melamine of two parts of 1.5g and the NaOH of 0.125g, 7.5g sodium chloride, 7.5g lithium chloride is respectively added again in two increment product, raw material is ground 10 ~ 30min in mortar, after fully mixing, be placed in crucible, with aluminium-foil paper, crucible oral area is sealed, be placed in Muffle furnace be warming up to 550 DEG C and be incubated 4h, powder mortar after sintering is levigate, by washed with de-ionized water and suction filtration be separated, separating obtained sample is dry 4h at 80 DEG C, obtains yellow receiving bore carbonitride.Contrast known by the product test result of the present embodiment and embodiment 4, when alkali metal chloride becomes sodium chloride from potassium chloride, the crystallinity deterioration of product, specific area die-offs; When alkali metal chloride is lithium chloride, suitable when the crystallinity of product and specific area and alkali metal chloride are potassium chloride.
Embodiment 6
The kind of alkali is on the impact of product: take the melamine of three parts of 1.5g and the potassium chloride of 7.5g, 0.14g potassium hydroxide, 0.06g lithium hydroxide, 0.26g strontium hydroxide is added again in three increment product, raw material is ground 10 ~ 30min in mortar, after fully mixing, be placed in crucible, with aluminium-foil paper, crucible oral area is sealed, be placed in Muffle furnace be warming up to 550 DEG C and be incubated 4h, powder mortar after sintering is levigate, by washed with de-ionized water and suction filtration be separated, separating obtained sample is dry 4h at 80 DEG C, obtains yellow receiving bore carbonitride.Contrast known by the product test result of the present embodiment and embodiment 3, alkali kind affects little on the specific area of product and crystallinity.
Embodiment 7
Receiving bore carbonitride photocatalytic degradation gaseous-phase organic pollutant isopropyl alcohol: be evenly pave in 32mm circular quartz groove in internal diameter by the receiving bore carbonitride sample dispersion of 50mg, is placed in above-mentioned quartz cell the closed container that volume is 0.5L, with artificial air (N
2: O
2=4:1, CO
2<1ppm) to above-mentioned quartz container purge 5 ~ 7min, to remove the CO in container
2injecting 400 μm of ol isopropyl alcohols, using 300W xenon lamp as light source, is the filter plate elimination ultraviolet light of 400nm by cutoff wavelength, during light-catalyzed reaction, from reactor, respectively get assay products composition in the gas inject gas chromatograph (Shimadzu GC-2014) of 0.5mL every 10min.
Under the above-described reaction conditions, when 60 minutes, gaseous state isopropyl alcohol is degradable, and mineralization rate reaches 23%.
Embodiment 8
Receiving bore carbonitride photocatalytic degradation gaseous-phase organic pollutant acetaldehyde: be evenly pave in 32mm circular quartz groove in internal diameter by the receiving bore carbonitride sample dispersion of 50mg, is placed in above-mentioned quartz cell the closed container that volume is 0.5L, with artificial air (N
2: O
2=4:1, CO
2<1ppm) to above-mentioned quartz container purge 5 ~ 7min, to remove the CO in container
2injecting 15 μm of ol acetaldehyde, using 300W xenon lamp as light source, is the filter plate elimination ultraviolet light of 400nm by cutoff wavelength, during light-catalyzed reaction, from reactor, respectively get assay products composition in the gas inject gas chromatograph (Shimadzu GC-2014) of 0.5mL every 10min.
Under the above-described reaction conditions, when 60 minutes, gaseous acetaldehyde is degradable, and mineralization rate reaches 86%.
Under same test condition, other organic pollution of receiving bore carbonitride photocatalytic degradation such as acetone, benzene, acetic acid are also evaluated, and result as shown in appendix 1.
The various organic pollution performance comparison of carbonitride photocatalytic degradation prepared by the receiving bore carbonitride of preparation in table 1 embodiment 1 and conventional method
1degradation rate: 1-pollutant remaining quantity/pollutant injection rate * 100%.
2mineralization rate: carbon dioxide generation/(pollutant injection rate * N) * 100%, [N refers to the number of pollutant carbon atoms].
3reaction condition: 300W xenon lamp (cutoff wavelength 400nm filter plate), 50mg sample, reaction time 60min.
By above embodiment, applicant lists the example of the preparation process of surface hydroxylation receiving bore carbonitride catalysis material and the application in light degradation gaseous-phase organic pollutant.The foregoing is only preferred embodiment of the present invention; protection scope of the present invention is not limited to above-mentioned case study on implementation; all equalizations done according to the present patent application the scope of the claims change and modify; all should belong to covering scope of the present invention, the protection domain required by the application is as shown in the application's claims.
Claims (10)
1. a surface hydroxylation receiving bore carbonitride catalysis material, is characterized in that, the nano pore structure of described catalysis material is the mesoporous of 5 ~ 30nm based on aperture, and is less than the micropore of 2nm containing aperture, and specific area is 10 ~ 90m
2/ g, surface graft has oh group.
2. a preparation method for surface hydroxylation receiving bore carbonitride catalysis material, is characterized in that, with melamine, alkali metal chloride and alkali for raw material, one-step method directly obtains the receiving bore carbonitride of surface hydroxylation.
3. the preparation method of surface hydroxylation receiving bore carbonitride catalysis material according to claim 2, is characterized in that, comprise the steps:
(1) by the grinding of the mixture of melamine, alkali metal chloride and alkali evenly;
(2) mixture in step (1) be placed in crucible and close, in Muffle furnace, 400 ~ 600 DEG C process 2 ~ 4 hours;
(3) product in step (2) is dissolved in deionized water, stirs, suspension filter paper is carried out suction filtration washing, alkali metal chloride in recycle-water washing lotion, product is placed in baking oven dry, then grinds, obtain end product.
4. the preparation method of surface hydroxylation receiving bore carbonitride catalysis material according to claim 3, is characterized in that, in described step (1), alkali metal chloride is reaction promoter, comprises sodium chloride, potassium chloride or lithium chloride.
5. the preparation method of surface hydroxylation receiving bore carbonitride catalysis material according to claim 3, is characterized in that, in described step (1), alkali is the alkali of alkali metal containing or alkali earth metal, is pore creating material and the raw material producing surface hydroxyl.
6. the preparation method of surface hydroxylation receiving bore carbonitride catalysis material according to claim 5, is characterized in that, in described step (1), alkali is potassium hydroxide, NaOH, lithium hydroxide or strontium hydroxide.
7. the preparation method of surface hydroxylation receiving bore carbonitride catalysis material according to claim 3, it is characterized in that, in described step (1), the mass ratio of melamine and chloride salt is in 0.05 ~ 10 scope, and the quality of alkali is 0.5% ~ 3% of the gross mass of melamine and chloride salt.
8. the preparation method of surface hydroxylation receiving bore carbonitride catalysis material according to claim 7, is characterized in that, in described step (1), the mass ratio of melamine and chloride salt is 0.2.
9. the preparation method of surface hydroxylation receiving bore carbonitride catalysis material according to claim 3, is characterized in that, 550 DEG C of process 4 hours in Muffle furnace in described step (2).
10. the application of surface hydroxylation receiving bore carbonitride catalysis material in degrading gaseous-phase organic pollutant, is characterized in that, described gaseous-phase organic pollutant comprises alcohol, aldehyde, ketone, acid and aromatic compound.
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