CN104415786A - Method for quickly preparing quasi-graphite-structure carbon nitride material by adopting microwave heating - Google Patents
Method for quickly preparing quasi-graphite-structure carbon nitride material by adopting microwave heating Download PDFInfo
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Abstract
The invention relates to a quick, energy-saving and high-yield preparation method of quasi-graphite-structure carbon nitride catalysis materials and application of the materials, belonging to the field of preparation and application of catalysis materials. According to the preparation process, one or multiple nitrogen-rich small organic molecules of urea, melamine, thiourea, cyanamide, dicyanamide, cyanuric chloride and cyanuric acid is/are taken as raw materials, a simple metal substance, a metallic oxide, a metal sulfide and a metal chloride are taken as microwave absorbers, microwave is taken as a heating source, and under the condition of radiation of microwave, the quasi-graphite-structure carbon nitride material can be quickly prepared. The prepared carbon nitride material has a large specific area and crystallinity and has high photocatalytic water decomposition hydrogen production performance and organic pollutant degradation performance. The preparation method provided by the invention is short in time, small in energy consumption, high in production efficiency and simple in process, does not have harsh preparation conditions, is easy to operate and has wide application prospect.
Description
Technical field
The present invention relates to the material synthesis method that a kind of quick, energy-conservation and high yield quantizes to prepare graphite-like structure carbonitride, belong to catalysis material preparations and applicatio technical field.
Background technology
Energy shortage and environmental pollution have become the global problem of restriction human social.Photocatalysis science can directly utilize decomposing water with solar energy hydrogen manufacturing and degradable organic pollutant, there are the potentiality of satisfied following large-scale industry hydrogen and solution problem of environmental pollution, being called as " engineering of dream ", is that the mankind have great expectations of one of final approach of the energy that solution faces at present and environmental problem.Since this technology finds from 1972, developed country between east and west has all dropped into substantial contribution and manpower, and photocatalysis science is developed rapidly.
More than ten years in past three, the research of domestic and international catalysis material mainly collects TiO2, on the metal oxides such as CdS and metal sulfide material.Metallic catalysis material not only price is relatively costly, and the secondary pollution problem of metal ion in photocatalysis is anti-caused by catalysis material instability, also significantly limit the actual application value of this kind of material.
2009, the people such as Wang again novelty the carbon nitride material of graphite-like structure is applied to photocatalysis field, thus make catalysis material be extended to metal-free catalysis material system by traditional metallic catalysis material system.Carbon nitride material has 1 as catalysis material) raw material are cheap at the rich content of occurring in nature; 2) high heat endurance and chemical stability; 3) narrow optical band gap, and the evident characteristic such as suitable conduction band and valence band location, thus make carbon nitride material in the research of photocatalysis science, be subject to increasing attention.
At present, carbon nitride material mainly through rich nitrogen organic molecule, as urea, melamine etc., high-temperature hot polymerizing technology preparation.The temperature of preparation is 400-600 DEG C, and the time is not from several hours to several days etc.Above-mentioned technique very time consumption and energy consumption, for meeting the demand of futurity industryization application, developing a kind of quick, energy-conservation technique efficiently preparing carbonitride, just seeming very urgent.
Summary of the invention
For the time consumption and energy consumption preparing graphite-like structure carbon nitride material at present, this invention exploits a kind of quick, energy-conservation new technology efficiently preparing carbon nitride material.The method not only technique is simple, easy to operate, and prepared carbonitride has higher photocatalytic hydrogen production by water decomposition performance and degradable organic pollutant performance.Therefore, the research of the present invention to the photocatalysis performance of carbon nitride material is significant.
The content that this technique is concrete is as follows: with rich nitrogen organic molecule for presoma, with simple substance/metal oxide/metal sulfide/metal chloride for microwave absorbing material, and be heating source with microwave, whole course of reaction only less than 20 minutes, thus need realize the efficient preparation fast of carbon nitride material.Importantly, prepared carbon nitride material has larger specific area and good photocatalysis property.
Wherein said rich nitrogen organic molecule comprises urea, melamine, thiocarbamide, cyanamide, cdicynanmide, Cyanuric Chloride, cyanuric acid organic precursor.The consumption of organic precursor is 100 milligrams only tens grams.
Wherein said microwave absorbing material is as follows: metal simple-substance element comprises Al, C (unformed phase), C (graphite-phase), Co, Fe, Mo, V, W, Zn; Metal oxide comprises Co
2o
3, CuO, Fe
3o
4, MnO
2, NiO, V
2o
5, WO
3; Metal sulfide comprises Cu
2s, FeS
2, MoS
2; Metal chloride comprises CuCl, ZnCl
2.
The large I of microwave power wherein for reacting is from 250W to 1000W;
Wherein said photocatalysis property comprises photocatalytic hydrogen production by water decomposition performance and to methyl orange, methylene blue, rhodamine B, phenol, p-nitrophenol organic pollution.
In a preferred embodiment, get the alumina crucible that 25mL put into by 6g urea, and cover the crucible of this 25mL mouth to mouth with the alumina crucible of a 50mL, seal the junction of two crucibles subsequently with alumina silicate felt.Inserted by the crucible that urea is housed sealed in the large alumina crucible with 200mL, buried by the crucible that urea is housed subsequently with cupric oxide, react 18 minutes under the microwave power of 1000W, the crucible of burying is taken out in cooling afterwards, can obtain carbon nitride material.Photocatalysis hydrogen production and degraded methyl orange result show, the carbonitride obtained has good photocatalysis property.
The present invention thus microwave reactor sampling market sale household microwave oven can realize this reaction.
In sum, content of the present invention is mainly as follows:
1. invented a kind of high efficiency preparation method of quick, energy-conservation synthesis carbonitride, described method is as follows: with rich nitrogen organic molecule for presoma, with simple substance element, metal oxide, metal sulfide, metal chloride for microwave absorbing material, and be heating source with microwave, whole course of reaction only needs 20 minutes, can realize the efficient preparation fast of carbon nitride material.
2. the method according to the 1st, wherein said rich nitrogen organic molecule comprises urea, melamine, thiocarbamide, cyanamide, cdicynanmide, Cyanuric Chloride, cyanuric acid organic precursor.
3. the metal simple-substance element described in claims 1 comprises Al, C (unformed phase), C (graphite-phase), Co, Fe, Mo, V, W, Zn; Metal oxide comprises Co
2o
3, CuO, Fe
3o
4, MnO
2, NiO, V
2o
5, WO
3; Metal sulfide comprises Cu
2s, FeS
2, MoS
2; Metal chloride comprises CuCl, ZnCl
2.
4. the method according to the 1st, the large I of the microwave power wherein for reacting is from 250W to 1000W.
5. the method according to the 1st, wherein said photocatalysis property comprises photocatalytic hydrogen production by water decomposition performance and to methyl orange, methylene blue, rhodamine B, phenol, p-nitrophenol organic pollution.
Accompanying drawing explanation
Below in conjunction with in the detailed description of accompanying drawing, above-mentioned feature and advantage of the present invention will be more obvious, wherein
Fig. 1, the carbon nitride material (a) that heating using microwave urea is prepared fast is polymerized the XRD diffracting spectrum of the carbon nitride material that urea (550 DEG C, 6h) obtains with traditional heating.The intensity of the XRD diffraction maximum of the carbonitride prepared by this technique obviously strengthens.
Fig. 2, the carbon nitride material (a) that heating using microwave urea is prepared fast is polymerized the FT-IR collection of illustrative plates of the carbon nitride material that urea (550 DEG C, 6h) obtains with traditional heating.
Fig. 3, the carbon nitride material (a) that heating using microwave urea is prepared fast is polymerized the physical absorption collection of illustrative plates of the carbon nitride material that urea (550 DEG C, 6h) obtains with traditional heating.Carbonitride prepared by this technique has larger specific area.
The carbon nitride material (a) that Fig. 4 heating using microwave urea is prepared fast is polymerized the photolysis water hydrogen performance of the carbon nitride material that urea (550 DEG C, 6h) obtains with traditional heating.Carbonitride prepared by this technique has good hydrogen production by water decomposition performance.
The carbon nitride material (a) that Fig. 5 heating using microwave urea is prepared fast is polymerized the photo-catalytic degradation of methyl-orange performance of the carbon nitride material that urea (550 DEG C, 6h) obtains with traditional heating.Carbonitride prepared by this technique has degraded methyl orange property of pigment preferably.
The XRD diffracting spectrum of the carbon nitride material of preparation fast under Fig. 6 heating using microwave urea 660W microwave power.
The XRD diffracting spectrum of the carbon nitride material that Fig. 7 heating using microwave melamine is prepared fast.
The XRD diffracting spectrum of the carbon nitride material that Fig. 8 heating using microwave cyanamide is prepared fast.
The XRD diffracting spectrum of the carbon nitride material that Fig. 9 heating using microwave thiocarbamide is prepared fast.
Detailed description of the invention
The preparation technology rapidly and efficiently preparing carbon nitride material of the present invention is further described below by specific embodiment.Subordinate's embodiment is only not used in for illustration of the present invention and limits the scope of the invention.Meanwhile, the carbon nitride material prepared by traditional heating Urea Process is used as and compares.
Implementation process is further illustrated with nonlimiting examples below.
Embodiment 1: graphite-like structure carbon nitride material is prepared in heating using microwave fast
Take the alumina crucible that 25mL put into by 6g urea, and cover the crucible of this 25mL mouth to mouth with the alumina crucible of a 50mL, seal the junction of two crucibles subsequently with alumina silicate felt.Inserted by the crucible that urea is housed sealed in the large alumina crucible with 200mL, buried by the crucible that urea is housed subsequently with cupric oxide, react 18 minutes under the microwave power of 1000W, the crucible of burying is taken out in cooling afterwards, can obtain carbon nitride material.
As shown in Figure 1, the material prepared by explanation is carbonitride to the XRD diffracting spectrum of carbon nitride material prepared in the present embodiment.
As shown in Figure 2, describe prepared material is carbon nitride material to the infrared spectrogram (FT-IR) of carbon nitride material prepared in the present embodiment.
The physical absorption curve of carbon nitride material prepared in the present embodiment as shown in Figure 3, describes prepared carbon nitride material and has larger specific area.
The photolysis water hydrogen performance of carbon nitride material prepared in the present embodiment as shown in Figure 4, describes prepared carbon nitride material and has good photocatalytic hydrogen production by water decomposition performance.
The degraded methyl orange property of pigment of carbon nitride material prepared in the present embodiment as shown in Figure 5, describes the performance that prepared carbon nitride material has degraded methyl orange preferably.
Embodiment 2: graphite-like structure carbon nitride material is prepared in heating using microwave fast
Take the alumina crucible that 25mL put into by 6g urea, and cover the crucible of this 25mL mouth to mouth with the alumina crucible of a 50mL, seal the junction of two crucibles subsequently with alumina silicate felt.Inserted by the crucible that urea is housed sealed in the large alumina crucible with 200mL, buried by the crucible that urea is housed subsequently with cupric oxide, react 18 minutes under the microwave power of 660W, the crucible of burying is taken out in cooling afterwards, can obtain carbon nitride material.
As shown in Figure 6, the material prepared by explanation is carbonitride to the XRD diffracting spectrum of carbon nitride material prepared in the present embodiment.
Embodiment 3: graphite-like structure carbon nitride material is prepared in heating using microwave fast
Take the alumina crucible that 25mL put into by 3g melamine, and cover the crucible of this 25mL mouth to mouth with the alumina crucible of a 50mL, seal the junction of two crucibles subsequently with alumina silicate felt.Inserted by the crucible that urea is housed sealed in the large alumina crucible with 200mL, buried by the crucible that urea is housed subsequently with cupric oxide, react 15 minutes under the microwave power of 1000W, the crucible of burying is taken out in cooling afterwards, can obtain carbon nitride material.
As shown in Figure 7, the material prepared by explanation is carbonitride to the XRD diffracting spectrum of carbon nitride material prepared in the present embodiment.
Embodiment 4: graphite-like structure carbon nitride material is prepared in heating using microwave fast
Take the alumina crucible that 3g thiocarbamide puts into 25mL, and cover the crucible of this 25mL mouth to mouth with the alumina crucible of a 50mL, seal the junction of two crucibles subsequently with alumina silicate felt.Inserted by the crucible that urea is housed sealed in the large alumina crucible with 200mL, buried by the crucible that urea is housed subsequently with cupric oxide, react 15 minutes under the microwave power of 1000W, the crucible of burying is taken out in cooling afterwards, can obtain carbon nitride material.
As shown in Figure 8, the material prepared by explanation is carbonitride to the XRD diffracting spectrum of carbon nitride material prepared in the present embodiment.
Embodiment 5: graphite-like structure carbon nitride material is prepared in heating using microwave fast
Take the alumina crucible that 3g cyanamide puts into 25mL, and cover the crucible of this 25 mL mouth to mouth with the alumina crucible of a 50mL, seal the junction of two crucibles subsequently with alumina silicate felt.Inserted by the crucible that urea is housed sealed in the large alumina crucible with 200mL, buried by the crucible that urea is housed subsequently with cupric oxide, react 15 minutes under the microwave power of 1000W, the crucible of burying is taken out in cooling afterwards, can obtain carbon nitride material.
As shown in Figure 9, the material prepared by explanation is carbonitride to the XRD diffracting spectrum of carbon nitride material prepared in the present embodiment.
Claims (5)
1. quick, an energy-conservation and high yield quantizes the synthetic method preparing graphite-like structure carbonitride, be characterized in utilizing cheap rich nitrogen organic molecule to be raw material, with simple substance element, metal oxide, metal sulfide, metal chloride for microwave suction ripple medium, take microwave as heating source, whole preparation process only needs 20 minutes, and prepared carbonitride catalysis material has higher catalytic performance, comprise photocatalytic hydrogen production by water decomposition performance and degraded organic contamination performance.
2. the rich nitrogen organic molecule described in claim 1 comprises urea, melamine, thiocarbamide, cyanamide, cdicynanmide, Cyanuric Chloride, cyanuric acid.
3. the metal simple-substance element described in claims 1 comprises Al, C (unformed phase), C (graphite-phase), Co, Fe, Mo, V, W, Zn; Metal oxide comprises Co
2o
3, CuO, Fe
3o
4, MnO
2, NiO, V
2o
5, WO
3; Metal sulfide comprises Cu
2s, FeS
2, MoS
2; Metal chloride comprises CuCl, ZnCl
2.
4. the microwave power size in claim 1 is from 250W to 1000W.
5. the organic pollution in claim 1 comprises methyl orange, methylene blue, rhodamine B, phenol and p-nitrophenol.
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| CN105731397A (en) * | 2014-12-10 | 2016-07-06 | 中国科学院大连化学物理研究所 | A preparing method of a nitrogen carbide material |
| CN105752953A (en) * | 2016-01-29 | 2016-07-13 | 张家港市东大工业技术研究院 | Preparation method of graphite phase carbonitride |
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| CN115445597A (en) * | 2022-08-12 | 2022-12-09 | 青岛科技大学 | Preparation method for reconstructing iodine-doped carbon nano tube in microwave environment and iodine-doped carbon nano tube |
| CN115318327A (en) * | 2022-08-17 | 2022-11-11 | 中化学朗正环保科技有限公司 | Preparation method of heterogeneous catalyst for treating near-neutral organic wastewater |
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