CN105688964A - Method for preparing graphite-shaped carbon nitride metal ion compound in ultrasonic field - Google Patents
Method for preparing graphite-shaped carbon nitride metal ion compound in ultrasonic field Download PDFInfo
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- CN105688964A CN105688964A CN201510955184.1A CN201510955184A CN105688964A CN 105688964 A CN105688964 A CN 105688964A CN 201510955184 A CN201510955184 A CN 201510955184A CN 105688964 A CN105688964 A CN 105688964A
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- carbon nitride
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
Abstract
The invention discloses a method for preparing a graphite-shaped carbon nitride metal ion compound in an ultrasonic field. According to the method, graphite-shaped carbon nitride and a metal ion compound thereof are rapidly synthesized on the condition that the ultrasonic field exists, and the whole synthesizing process lasts for about 30 min; the formed graphite-shaped carbon nitride (g-C3N4) metal ion compound (M<+>-g-C3N4) is good in uniformity and dispersity and has high catalytic activity, and the degradation rate of the compound to MO can reach 98.5% or above. The method has the advantages that the reaction time is short, the reaction conditions are mild, the efficiency of the obtained product on degrading contaminants is high, and the reaction speed is high, and the method has a certain application prospect.
Description
[technical field]
The invention belongs to field of composite material preparation, be specifically related to a kind of method preparing graphitic carbon nitride metal ion complex under ultrasonic field。
[background technology]
At present, graphite shape carbon nitride material synthesizes mainly through hydrothermal synthesis method, thermal decomposition method, high temperature and high pressure method and masterplate method。Solvent-thermal method refers in special closed reactor (Hydrothermal Synthesis still and autoclave), utilize the organic solvents such as benzene, methanol, ethanol, DMF, chloroform, carbon tetrachloride as reactant or medium, adopt and be similar to the newly-designed synthetic method of hydro-thermal ratio juris。Have the unexistent plurality of advantages of conventional synthesis method, as be conducive to high purity material synthesis, suitable in wide range, the existence of surface hydroxyl can be effectively prevented from, there is the feature of low temperature, high pressure, but there is also response time long shortcoming；Masterplate synthetic method is exactly a kind of synthetic method controlling, affect, modify and constructing the character of target substance (synthetic product), pattern and structure with the material (i.e. masterplate) with particular space structure and group。There is the features such as simple to operate, easy control of reaction system, easy doping, but the shortcoming such as the subsequent treatment process that there is masterplate is complicated；Thermal decomposition method is exactly that the precursor compound of powder body is heated method under certain condition that make it decompose and to prepare powder body。This method has the features such as simple and reliable, easy operation, but there is also the shortcomings such as restricted application。
It is known that photocatalysis technology is because it has low energy consumption and can utilize solar energy simultaneously, the excellent feature such as easily operation, simple, the non-secondary pollution of consersion unit and become the new power-saving technology and environmental improvement technology that there are broad prospect of application。But, greatly have impact on its commercialization promote because there are the fatal defects of two comparisons, one is that quantum efficiency is low, because light-catalysed photo-generate electron-hole is higher and cause that photocatalysis performance does not highlight to recombination rate, have impact on actually used economy；Two is that sunlight utilization rate is too low, or because photoresponse narrow limits, or because absorption intensity is not high, and cause arriving photocatalyst surface, can be effective to excite photoelectronic photon very few。Graphitic carbon nitride also has disadvantages mentioned above as novel nonmetal photocatalytic semiconductor, thus its catalytic performance is not efficient, therefore extremely it is necessary, to its target being modified reaching enhancing photocatalysis performance, to lay a solid foundation for its practical application in the future。Industry thus attempt it is carried out modification, currently mainly have following methods: noble metal loading, ion doping (including transition metal, nonmetallic ion), dye photoactivation and semiconductors coupling etc.。These methods each have feature and the advantage of oneself, but there is the drawbacks such as response time length or severe reaction conditions, and therefore, reaction time consumption is short, and the method for modifying of energy consumption low condition gentleness is particularly necessary。
[summary of the invention]
It is an object of the invention to overcome above-mentioned deficiency, a kind of method preparing graphitic carbon nitride metal ion complex under ultrasonic field is provided, prior art preparation time length, condition is overcome to require high defect, having the ability of decomposing organic pollutant higher, preparation and application to carbon nitride material have important function。
In order to achieve the above object, the present invention comprises the following steps:
Step one, is dispersed in solvent medium according to molal weight by 1 part of graphitic carbon nitride, obtains solution A；
The slaines of 2～5 parts are dissolved in solution A by step 2, are placed in ultrasonic reactor, are cooled to room temperature after ultrasonic reaction；
Step 3, by the solution sucking filtration after cooling, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally uses distilled water cyclic washing for several times until filtrate is neutral again, obtains substance C；
Step 4, dries in a vacuum by substance C, collects grinding after drying, namely obtains graphitic carbon nitride metal ion complex。
In described step one, the volume ratio of carbonitride quality and solvent medium is 1:30。
In described step one, solvent medium includes the one of water, ethanol, methanol, acetonitrile。
In described step one, dispersion adopts ultrasonic disperse, and ultrasonic time is 30min。
In described step 2, slaine comprises the one in copper nitrate, copper sulfate, copper chloride, iron sulfate, ferric nitrate, iron chloride, silver nitrate, silver acetate。
In described step 2, ultrasonic power is 200-500W, and reaction temperature is maintained at 120～180 DEG C, response time 5-15min。
In described step 4, vacuum drying dries 12 hours at 55 DEG C。
Compared with prior art, graphitic carbon nitride of the present invention and metal ion complex thereof all synthesize rapidly under ultrasound field existent condition, and whole building-up process lasts about 30 minutes；Graphitic carbon nitride (the g-C formed3N4) metal ion complex (M+-g-C3N4) uniformity and dispersibility be better, has higher catalysis activity, to the degradation rate of MO up to more than 98.5%, it is short that this method has the response time, and reaction condition is gentle, and products therefrom degradation of contaminant efficiency is high, the features such as response speed is fast, have certain application prospect。
[accompanying drawing explanation]
Fig. 1 is the X-ray diffractogram of catalysis material of the present invention；Wherein, a is iron ion carbonitride (g-C3N4) catalysis material, b is iron ion carbonitride complex (Fe3+-g-C3N4) catalysis material, c is copper ion carbonitride complex (Cu2+-g-C3N4) catalysis material, d is silver ion carbonitride complex (Ag+-g-C3N4) catalysis material；
Fig. 2 is iron ion carbonitride complex (Fe3+-g-C3N4) the x-ray photoelectron energy spectrogram of catalysis material；
Fig. 3 is copper ion carbonitride complex (Cu2+-g-C3N4) the x-ray photoelectron energy spectrogram of catalysis material。
Fig. 4 is silver ion carbonitride complex (Ag+-g-C3N4) the x-ray photoelectron energy spectrogram of catalysis material。
Fig. 5 is the UV-vis DRS spectrogram of catalysis material of the present invention；Wherein, a is iron ion carbonitride complex (Fe3+-g-C3N4) catalysis material, b is silver ion carbonitride complex (Ag+-g-C3N4) catalysis material, c is copper ion carbonitride complex (Cu2+-g-C3N4) catalysis material, d is carbonitride (g-C3N4) catalysis material；
Fig. 6 is the physical absorption figure of catalysis material of the present invention；Wherein, a is iron ion carbonitride complex (Fe3+-g-C3N4) catalysis material, b is silver ion carbonitride complex (Ag+-g-C3N4) catalysis material, c is copper ion carbonitride complex (Cu2+-g-C3N4) catalysis material；
Fig. 7 is the catalysis material of the present invention photocatalytic degradation curve chart to methyl orange；Wherein, a is carbonitride complex (g-C3N4) catalysis material, b is copper ion carbonitride complex (Cu2+-g-C3N4) catalysis material, c is silver ion carbonitride complex (Ag+-g-C3N4) catalysis material, d is iron ion carbonitride complex (Fe3+-g-C3N4) catalysis material。
[detailed description of the invention]
Below in conjunction with drawings and Examples, the present invention will be further described。
Embodiment 1:
Weigh carbonitride 0.5g and be scattered in 50mL deionized water, ultrasonic 30min；Separately weighing 2.5g iron chloride and be dissolved in above-mentioned solution, solution goes in the double-deck reaction bulb that capacity is 100mL。Open light source and arrange ultrasonic reactor program make reaction temperature be maintained at 120 DEG C reaction 3min, naturally cool to room temperature afterwards。React after terminating, the mixture sucking filtration that will generate, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally use distilled water cyclic washing for several times until filtrate is neutral again。The solid matter remained in funnel dried 12 hours in a vacuum at 55 DEG C and collects, putting into agate mortar grinding and preserve and obtain sample。
Embodiment 2:
Weigh carbonitride 0.75g and be scattered in 45mL ethanol, ultrasonic 30min；Separately weighing 3.0g copper sulfate and be dissolved in above-mentioned solution, solution goes in the double-deck reaction bulb that capacity is 100mL。Open light source and arrange ultrasonic reactor program make reaction temperature be maintained at 150 DEG C reaction 5min, naturally cool to room temperature afterwards。React after terminating, the mixture sucking filtration that will generate, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally use distilled water cyclic washing for several times until filtrate is neutral again。The solid matter remained in funnel dried 12 hours in a vacuum at 55 DEG C and collects, putting into agate mortar grinding and preserve and obtain sample。
Embodiment 3:
Weigh carbonitride 0.50g and be scattered in 60mL methanol, ultrasonic 30min；Separately weighing 1.5g silver nitrate and be dissolved in above-mentioned solution, solution goes in the double-deck reaction bulb that capacity is 100mL。Open light source and arrange ultrasonic reactor program make reaction temperature be maintained at 140 DEG C reaction 5min, naturally cool to room temperature afterwards。React after terminating, the mixture sucking filtration that will generate, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally use distilled water cyclic washing for several times until filtrate is neutral again。The solid matter remained in funnel dried 12 hours in a vacuum at 55 DEG C and collects, putting into agate mortar grinding and preserve and obtain sample。
Embodiment 4:
Weigh the graphitic carbon nitride (M of metal ion compound+/g-C3N4) each 0.5000g is put in beaker, add the methyl orange solution of 100mL80mg/L, ultrasonic 5min, before xenon lamp irradiates, first it is placed in dark and stirs 30min to reach adsorption equilibrium, sample 1mL at interval of 10min, after diluting 10 times with deionized water, centrifugal, take supernatant and load Pyrex bottle, labelling also deposits dark place with tinfoil parcel；Then under the irradiation of xenon lamp, carry out photocatalytic degradation test 6 hours, take 1ml solution every 10min, centrifugal after diluting 10 times, take supernatant under ultraviolet-uisible spectrophotometer, test the change of methyl orange dye concentration。
Embodiment 5:
Step one, is dispersed in acetonitrile according to molal weight by 1 part of graphitic carbon nitride, disperses ultrasonic disperse, and ultrasonic time is 30min, and the volume ratio making carbonitride quality and solvent medium is 1:30, obtains solution A；
The copper nitrates of 2～5 parts are dissolved in solution A by step 2, are placed in ultrasonic reactor, are cooled to room temperature after ultrasonic reaction, and ultrasonic power is 200W, and reaction temperature is maintained at 120 DEG C, response time 5min；
Step 3, by the solution sucking filtration after cooling, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally uses distilled water cyclic washing for several times until filtrate is neutral again, obtains substance C；
Step 4, dries substance C 12 hours in the vacuum of 55 DEG C, collects grinding after drying, namely obtain graphitic carbon nitride metal ion complex。
Embodiment 6:
Step one, disperses 1 part of graphitic carbon nitride in deionized water according to molal weight, disperses ultrasonic disperse, and ultrasonic time is 30min, and the volume ratio making carbonitride quality and solvent medium is 1:30, obtains solution A；
The copper chlorides of 3 parts are dissolved in solution A by step 2, are placed in ultrasonic reactor, are cooled to room temperature after ultrasonic reaction, and ultrasonic power is 500W, and reaction temperature is maintained at 180 DEG C, response time 15min；
Step 3, by the solution sucking filtration after cooling, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally uses distilled water cyclic washing for several times until filtrate is neutral again, obtains substance C；
Step 4, dries substance C 12 hours in the vacuum of 55 DEG C, collects grinding after drying, namely obtain graphitic carbon nitride metal ion complex。
Embodiment 7:
Step one, disperses 1 part of graphitic carbon nitride in ethanol according to molal weight, disperses ultrasonic disperse, and ultrasonic time is 30min, and the volume ratio making carbonitride quality and solvent medium is 1:30, obtains solution A；
Step 2, by the ferric sulfate solution of 4 parts in solution A, is placed in ultrasonic reactor, is cooled to room temperature after ultrasonic reaction, and ultrasonic power is 350W, and reaction temperature is maintained at 150 DEG C, response time 10min；
Step 3, by the solution sucking filtration after cooling, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally uses distilled water cyclic washing for several times until filtrate is neutral again, obtains substance C；
Step 4, dries substance C 12 hours in the vacuum of 55 DEG C, collects grinding after drying, namely obtain graphitic carbon nitride metal ion complex。
Embodiment 8:
Step one, is dispersed in methanol according to molal weight by 1 part of graphitic carbon nitride, disperses ultrasonic disperse, and ultrasonic time is 30min, and the volume ratio making carbonitride quality and solvent medium is 1:30, obtains solution A；
The ferric nitrates of 5 parts are dissolved in solution A by step 2, are placed in ultrasonic reactor, are cooled to room temperature after ultrasonic reaction, and ultrasonic power is 400W, and reaction temperature is maintained at 130 DEG C, response time 8min；
Step 3, by the solution sucking filtration after cooling, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally uses distilled water cyclic washing for several times until filtrate is neutral again, obtains substance C；
Step 4, dries substance C 12 hours in the vacuum of 55 DEG C, collects grinding after drying, namely obtain graphitic carbon nitride metal ion complex。
Embodiment 9:
Step one, is dispersed in acetonitrile according to molal weight by 1 part of graphitic carbon nitride, disperses ultrasonic disperse, and ultrasonic time is 30min, and the volume ratio making carbonitride quality and solvent medium is 1:30, obtains solution A；
The silver acetates of 4 parts are dissolved in solution A by step 2, are placed in ultrasonic reactor, are cooled to room temperature after ultrasonic reaction, and ultrasonic power is 400W, and reaction temperature is maintained at 160 DEG C, response time 14min；
Step 3, by the solution sucking filtration after cooling, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally uses distilled water cyclic washing for several times until filtrate is neutral again, obtains substance C；
Step 4, dries substance C 12 hours in the vacuum of 55 DEG C, collects grinding after drying, namely obtain graphitic carbon nitride metal ion complex。
Claims (7)
1. the method preparing graphitic carbon nitride metal ion complex under ultrasonic field, it is characterised in that comprise the following steps:
Step one, is dispersed in solvent medium according to molal weight by 1 part of graphitic carbon nitride, obtains solution A；
The slaines of 2～5 parts are dissolved in solution A by step 2, are placed in ultrasonic reactor, are cooled to room temperature after ultrasonic reaction；
Step 3, by the solution sucking filtration after cooling, then successively with water, ethanol cyclic washing solid product, to remove by-product and other impurity that reaction generates, finally uses distilled water cyclic washing for several times until filtrate is neutral again, obtains substance C；
Step 4, dries in a vacuum by substance C, collects grinding after drying, namely obtains graphitic carbon nitride metal ion complex。
2. the method preparing graphitic carbon nitride metal ion complex under ultrasonic field according to claim 1, it is characterised in that in described step one, the volume ratio of carbonitride quality and solvent medium is 1:30。
3. the method preparing graphitic carbon nitride metal ion complex under ultrasonic field according to claim 1, it is characterised in that in described step one, solvent medium includes the one of water, ethanol, methanol, acetonitrile。
4. the method preparing graphitic carbon nitride metal ion complex under ultrasonic field according to claim 1, it is characterised in that in described step one, dispersion adopts ultrasonic disperse, and ultrasonic time is 30min。
5. the method preparing graphitic carbon nitride metal ion complex under ultrasonic field according to claim 1, it is characterized in that, in described step 2, slaine comprises the one in copper nitrate, copper sulfate, copper chloride, iron sulfate, ferric nitrate, iron chloride, silver nitrate, silver acetate。
6. the method preparing graphitic carbon nitride metal ion complex under ultrasonic field according to claim 1, it is characterised in that in described step 2, ultrasonic power is 200-500W, and reaction temperature is maintained at 120～180 DEG C, response time 5-15min。
7. the method preparing graphitic carbon nitride metal ion complex under ultrasonic field according to claim 1, it is characterised in that in described step 4, vacuum drying dries 12 hours at 55 DEG C。
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| CN106745469A (en) * | 2016-11-23 | 2017-05-31 | 山西大学 | A kind of method of direct utilization solar radiation photocatalytic degradation phthalic acid ester pollutant |
| CN116273051A (en) * | 2023-03-21 | 2023-06-23 | 榆林学院 | Gamma-Al 2 O 3 Supported ruthenium-nickel catalyst and application thereof in phenol hydrogenation reaction |
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| CN106745469B (en) * | 2016-11-23 | 2019-05-14 | 山西大学 | A kind of direct method using solar radiation photocatalytic degradation phthalic acid ester pollutant |
| CN116273051A (en) * | 2023-03-21 | 2023-06-23 | 榆林学院 | Gamma-Al 2 O 3 Supported ruthenium-nickel catalyst and application thereof in phenol hydrogenation reaction |
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Application publication date: 20160622 |