CN113666345B - Preparation method and application of graphite oxide phase carbon nitride - Google Patents
Preparation method and application of graphite oxide phase carbon nitride Download PDFInfo
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- CN113666345B CN113666345B CN202111025897.XA CN202111025897A CN113666345B CN 113666345 B CN113666345 B CN 113666345B CN 202111025897 A CN202111025897 A CN 202111025897A CN 113666345 B CN113666345 B CN 113666345B
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 63
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 46
- 239000010439 graphite Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 20
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000003647 oxidation Effects 0.000 claims abstract description 19
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000003381 stabilizer Substances 0.000 claims abstract description 9
- 238000005119 centrifugation Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 28
- 239000002244 precipitate Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 239000006228 supernatant Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 12
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 6
- 239000004317 sodium nitrate Substances 0.000 claims description 6
- 235000010344 sodium nitrate Nutrition 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 15
- 230000002776 aggregation Effects 0.000 abstract description 11
- 238000005054 agglomeration Methods 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 230000003313 weakening effect Effects 0.000 abstract description 3
- 239000012876 carrier material Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- 229910052760 oxygen Inorganic materials 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000012286 potassium permanganate Substances 0.000 description 9
- 239000005457 ice water Substances 0.000 description 8
- 239000007800 oxidant agent Substances 0.000 description 8
- 230000001590 oxidative effect Effects 0.000 description 8
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 7
- 239000002356 single layer Substances 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 125000003700 epoxy group Chemical group 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
Abstract
The invention discloses a preparation method of graphite oxide phase carbon nitride, which comprises the steps of dispersing graphite phase carbon nitride and an oxidation promoter in mixed acid liquid at low temperature, and adding an oxidation stabilizer; then a small amount of potassium ferrate is added for many times; finally, obtaining graphite oxide phase carbon nitride after centrifugation, standing, washing and drying. The graphite oxide phase carbon nitride prepared by the method has the advantages of good dispersibility, good stability, good nanoparticle carrying effect, weakening of nanoparticle agglomeration, environmental protection of the preparation process and safety effect; the invention also provides application of the graphite oxide phase carbon nitride prepared by the method based on the same inventive concept, and the graphite oxide phase carbon nitride can be widely applied to the field of carrier materials of nano particles.
Description
Technical Field
The invention relates to the field of material preparation, in particular to a preparation method and application of graphite oxide phase carbon nitride.
Background
Graphite phase carbon nitride (g-C) 3 N 4 ) Is a carbon nitrogen compound having a general formula close to C 3 N 4 Because of the unique single-layer six-membered ring network structure, the nano particles can grow into nano microcrystals in situ from quantum dots on the nodes of the single-layer six-membered ring network structure, so that the nano particles are widely used as carrier materials of the nano particles by graphite-phase carbon nitride, but the nano particles have a plurality of limitations in practical application. Because the graphite phase carbon nitride sheets are tightly combined and have smaller surface area, the adsorption coverage rate of metal ions is insufficient, the nano metal ions are not convenient to load, and the metals with dispersed atoms on the graphite phase carbon nitride are unstable in thermodynamics and are easy to aggregate to form clusters.
And oxidized graphite-phase carbon nitride (g-C) 3 N 4 ) Namely, graphite-phase carbon nitride, can solve the problem of the graphite-phase carbon nitride (g-C 3 N 4 ) The carrying effect is poor and the agglomeration is easy to occur due to the self structure. The graphite oxide phase carbon nitride has a unique single-layer six-membered ring network structure, can be used as a carrier matrix material and is used as an excellent carrier of nano particles. Because the oxidized graphite phase carbon nitride has hydrophilic oxygen-containing groups, the water solubility of the graphite phase carbon nitride is improved, the solubility of the oxidized carbon nitride in water is increased, the dispersion effect is good, and the stability is increased; meanwhile, the introduced oxygen-containing groups enlarge interlayer spacing due to steric hindrance effect, so that the interlayer agglomeration phenomenon is reduced.
However, in the process of preparing the graphite-phase carbon nitride, the graphite-phase carbon nitride generally adopts potassium permanganate as an oxidant, and the complete six-membered ring network structure of the graphite-phase carbon nitride is easily damaged partially in the process of oxidizing the carbon nitride, so that oxygen-containing functional groups (hydroxyl groups and epoxy groups) of the graphite-phase carbon nitride are reduced, and carbonyl defect areas are increased, so that the oxidized graphite-phase carbon nitride is poor in carrying effect and easy to agglomerate; and chemical residues adhering to the surface of the carbon nitride are also difficult to remove. And the manganese ions generated in the oxidation process of potassium permanganate can cause serious heavy metal pollution, and safety accidents such as explosion and the like easily occur in the reaction process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method and the application of the graphite oxide phase carbon nitride, which have the advantages of good dispersibility, good stability, good nanoparticle carrying effect, weakening of nanoparticle agglomeration, environmental protection and safety in the preparation process.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of graphite oxide phase carbon nitride comprises the following steps:
s1: adding 4×10 in mass fraction into a reaction vessel 4 -9×10 4 Mixing the acid solution, and cooling to below 10 ℃; then adding 1×10 respectively 3 -1.5×10 3 Part graphite phase carbon nitride and 0.5 x 10 3 -1.5×10 3 The oxidation promoter is added and fully stirred to be uniformly dispersed; finally, adding 1-5 parts of oxidation stabilizer, and fully stirring to uniformly disperse the oxidation stabilizer to obtain solution A;
s2: maintaining the temperature below 10 ℃ and adding 3X 10 to the solution A by mass fraction 3 -5×10 3 Potassium ferrate is added and fully stirred for 1.5-2h; heating to 25-35deg.C, adding 2×10 3 -4×10 3 Potassium ferrate is added and fully stirred for 2-3h; finally, heating to 45-50 ℃ and stirring for 1.5-2h to obtain a solution B;
s3: centrifuging the solution B obtained in the step S2, standing to obtain supernatant and precipitate, and washing the precipitate with pure water; repeating the above centrifugation, standing, and washing until the pH of the supernatant is 6.5-7.5, to obtain final precipitate.
S4: and (3) freeze-drying the final precipitate obtained in the step (S3) by a vacuum freeze dryer to obtain graphite oxide phase carbon nitride.
Further, in the step S1, the mixed acid liquid is a mixed solution of sulfuric acid and hydrochloric acid, wherein the mass ratio of the sulfuric acid to the hydrochloric acid is 30:1-70:1.
Further, in S1, the oxidation stabilizer is at least one of periodic acid and citric acid.
Further, in S1, the oxidation stabilizer is preferably a mixture of periodic acid and citric acid, wherein the mass ratio of periodic acid to citric acid is 1:2-2:1.
In the step S1, the oxidation promoter is at least one of sodium nitrate and potassium nitrate.
Further, in S1, the potassium ferrate is added at two different temperatures by adopting a method of small eating amount to prevent the potassium ferrate from bursting, and when the system generates bubbles and the color changes to brown black, the adding speed of the potassium ferrate is indicated to be too fast, and the adding speed of the potassium ferrate should be properly slowed down.
In S3, the rotation speed adopted in the centrifugation is 7000-10000rpm, and the centrifugation time is 30-60min.
Further, in S3, the standing time is 15-20min.
Further, in S3, the amount of pure water used in the washing process is 5X 10 in parts by mass 4 Parts by weight.
Based on the same inventive concept, the invention also provides an application of the graphite oxide phase carbon nitride prepared by the preparation method, wherein the graphite oxide phase carbon nitride is used for carrying nano particles.
Further, the graphite oxide phase carbon nitride is used for carrying silver nanoparticles.
In the invention, graphite-phase carbon nitride is oxidized by a strong oxidant to obtain graphite-phase carbon nitride oxide; because the introduced oxygen-containing group is hydrophilic, the water solubility of graphite phase carbon nitride is improved, so that the solubility of oxidized carbon nitride in water is increased, the dispersion effect is good, and the stability is increased; meanwhile, the introduced oxygen-containing groups enlarge interlayer spacing due to steric hindrance effect, so that the interlayer agglomeration phenomenon is reduced.
The reason why the graphite oxide phase carbon nitride can realize good dispersibility, weakening agglomeration and good nanoparticle carrying effect is that more oxygen-containing groups (hydroxyl groups, epoxy groups and the like) are introduced into the oxidized single-layer six-membered ring network structure, the hydrophilicity of the oxygen-containing groups and larger steric hindrance can enhance the dispersibility of the graphite oxide phase carbon nitride and weaken the agglomeration phenomenon of the graphite phase carbon nitride; the more carbonyl defect areas are not beneficial to loading and adsorbing the nano particles by graphite oxide phase carbon nitride, and the nano particles are unstable in thermodynamics due to carbonyl, so that the phenomena of difficult adsorption and unstable adsorption are caused; therefore, to realize good dispersibility, no agglomeration, good nanoparticle carrying effect and stable carrying effect of the graphite oxide phase carbon nitride, more oxygen-containing groups (hydroxyl groups, epoxy groups and the like) and fewer carbonyl defect areas are introduced into the single-layer six-membered ring network structure.
The oxidant adopted by the invention is potassium ferrate instead of potassium permanganate in the prior art, so that the problems can be exactly solved; when potassium permanganate is used for oxidation, oxygen-containing functional groups (hydroxyl groups and epoxy groups) are more distributed at adjacent positions of the carbon layer plane, the network structure is more stable, and each sheet layer directly has strong acting force, so that the dispersion capability in water is poor and aggregation is easy. And potassium permanganate is a strong oxidant, has strong oxidation performance, and can generate peroxidation phenomenon, so that introduced oxygen-containing functional groups (hydroxyl and epoxy groups) are converted into carbonyl groups, and more carbonyl defect areas are generated, thereby being unfavorable for carrying and carrying stability of nano particles. The invention adopts potassium ferrate, the oxidation character is milder, and more oxygen-containing groups (hydroxyl, epoxy, etc.) and fewer carbonyl defect areas can be introduced into the single-layer six-membered ring net-shaped structure under the same oxidation effect. Meanwhile, the effects of good dispersibility, no agglomeration, good nanoparticle carrying effect and stable carrying performance of the graphite oxide phase carbon nitride are realized. And the whole process has higher yield.
Compared with the prior art, the invention has the beneficial effects that: 1. compared with the graphite oxide phase carbon nitride prepared by taking potassium permanganate as an oxidant, the graphite oxide phase carbon nitride prepared by taking potassium ferrate as the oxidant has better stability, better dispersibility and higher yield; 2. the graphite oxide phase carbon nitride prepared by the method has a complete and unique single-layer six-membered ring network structure, can better carry nano particles, and effectively avoids agglomeration of the nano particles. 3. The environment-friendly oxidant potassium ferrate is used, heavy metal ions cannot be generated, heavy metal pollution is caused, and meanwhile, the wastewater generated in the preparation process is relatively easy to treat. In the purification process, the washing times are less, the sewage is generated relatively less, and the method is suitable for industrial mass production; no chemical substance residue after purification and no potential harm to human health.
Drawings
FIG. 1 is a scanning electron microscope image of samples prepared in example 1 of the present invention at different magnifications.
Detailed Description
Example 1
S1: 60g of 98% concentrated sulfuric acid and 2g of concentrated hydrochloric acid are mixed and then poured into a reaction bottle, and the reaction bottle is placed into an ice water bath to be cooled to 6 ℃. Adding 1g of graphite phase carbon nitride and 1g of sodium nitrate into a reaction bottle, and fully stirring for 25 minutes to uniformly disperse the graphite phase carbon nitride and the sodium nitrate; finally, 0.001g of periodic acid and 0.002g of citric acid are added and stirred for 10min to obtain solution A.
S2: the ice water bath is kept at 10 ℃, 4g of potassium ferrate is slowly added into the solution A, and bubbles are avoided. Stirring was continued for 2h. 3g of potassium ferrate was added continuously in portions and stirred for 2h at 30 ℃. Heating to 45 ℃ and stirring for 2 hours to obtain a solution B.
S3: solution B was centrifuged at 10000rpm for 60min. Standing for layering for 20min, standing to obtain supernatant and precipitate, and pouring out supernatant. The precipitate was washed with 50g of pure water, and the above centrifugation, standing, and washing were repeated until the pH of the supernatant was 7.0, to obtain 2.95g of the final precipitate.
S4: and (3) freeze-drying the final precipitate obtained in the step (S3) by a vacuum freeze dryer to obtain 0.78g of graphite oxide phase carbon nitride.
Example 2
S1: 70g of 98% concentrated sulfuric acid and 1g of concentrated hydrochloric acid are firstly mixed and then poured into a reaction bottle, and the reaction bottle is placed into an ice water bath to be cooled to 8 ℃. Adding 1.5g of graphite phase carbon nitride and 0.8g of potassium nitrate into a reaction bottle, and fully stirring for 40 minutes to uniformly disperse the mixture; finally, 0.002g of periodic acid and 0.002g of citric acid are added and stirred for 15min to obtain solution A.
S2: the ice water bath is kept at 8 ℃, 5g of potassium ferrate is slowly added into the solution A, and bubbles are avoided. Stirring was continued for 2h. 3g of potassium ferrate was added in portions and stirred for 2.5h at 35 ℃. Heating to 50 ℃ and stirring for 1.5h to obtain a solution B.
S3: solution B was centrifuged at 9000rpm for 40min. Standing for layering for 20min, standing to obtain supernatant and precipitate, and pouring out supernatant. The precipitate was washed with 50g of pure water, and the above-mentioned centrifugation, standing, washing were repeated until the pH of the supernatant was 6.5, to obtain 3.89g of the final precipitate.
S4: and (3) freeze-drying the final precipitate obtained in the step (S3) by a vacuum freeze dryer to obtain 1.23g of graphite oxide phase carbon nitride.
Example 3
S1: 85g of 98% concentrated sulfuric acid and 1.5g of concentrated hydrochloric acid are firstly mixed and poured into a reaction bottle, and the reaction bottle is placed into an ice water bath to be cooled to 10 ℃. Adding 1.2g of graphite phase carbon nitride, 0.4g of sodium nitrate and 0.5g of potassium nitrate into a reaction bottle, and fully stirring for 40 minutes to uniformly disperse the materials; finally, 0.002g of periodic acid and 0.001g of citric acid are added and stirred for 10min to obtain solution A.
S2: the ice water bath is kept at 6 ℃, 3.5g of potassium ferrate is slowly added into the solution A, and bubbles are avoided. Stirring was continued for 2h. 2.9g of potassium ferrate was added in portions and stirred for 2-3h at 30 ℃. Heating to 45 ℃ and stirring for 1.5h to obtain a solution B.
S3: solution B was centrifuged at 8000rpm for 50min. Standing for layering for 15min, standing to obtain supernatant and precipitate, and pouring out supernatant. The precipitate was washed with 50g of pure water, and the above-mentioned centrifugation, standing, washing were repeated until the pH of the supernatant was 7.0, to obtain 2.87g of the final precipitate.
S4: and (3) freeze-drying the final precipitate obtained in the step (S3) by a vacuum freeze dryer to obtain 0.98g of graphite oxide phase carbon nitride.
Comparative example 1
1) 100g of 98% concentrated sulfuric acid is poured into a reaction bottle, and the reaction bottle is placed into an ice-water bath to be cooled to below 5 ℃. 1g of graphite phase carbon nitride and 1g of sodium nitrate are added into a reaction bottle, and are completely dissolved under stirring to obtain a solution A.
2) 4g of potassium permanganate is slowly added into the solution A at the temperature of 5 ℃ in an ice water bath for 1.5 hours, so that bubbles are avoided. Stirring was continued for 2h. Continuously adding 3g of potassium permanganate in batches, after adding the potassium permanganate for 1 hour, and stirring the mixture for 3 hours at 25-30 ℃. Heating to 50 ℃ and stirring for 2 hours to obtain a solution B.
3) 200g of 3% sulfuric acid solution was slowly added to the solution B, and stirring was continued for 2 hours after the addition of 0.5 hour. Then, 30g of pure water and 0.004g of citric acid were added, followed by adding 3g of hydrogen peroxide (28.5%) and stirring for 20min.
4) Centrifugal at 10000rpm for 30min. Standing for layering for 20min, and pouring out supernatant. 100g of pure water is added and stirred, and the mixture is washed for a plurality of times until the solution is neutral.
5) And (5) putting the sample into a vacuum freeze dryer for freeze drying to obtain the product.
Example 1 and comparative example 1 yield comparison
Table 1 comparison of example 1 and comparative example 1 yields
In Table 1, the parallels (1), (2) and (3) represent the repetition examples or comparative examples
As can be seen from Table 1, the yield of example 1 was higher than that of comparative example 1, and the distribution of the detected data was uniform. Example 1 the reaction was carried out at a lower temperature and the reaction time was significantly reduced, so the yield was relatively higher.
Example 1 and comparative example 1 sample Process hazard comparison
In example 1 and comparative example 1, 20 experiments were performed, and occurrence rates of events such as failure in temperature control and flash occurred.
Table 2 comparison of event occurrence rates for example 1 and comparative example 1
| Incidence of event | |
| Example 1 | 5％ |
| Comparative example 1 | 35％ |
As can be seen from table 2, comparative example 1 has a higher occurrence rate of events than example 1. Because the example 1 oxidizing agent uses potassium ferrate, the reaction process is relatively mild and easy to control.
Claims (3)
1. The application of the graphite oxide phase carbon nitride is characterized in that the graphite oxide phase carbon nitride is used for carrying nano particles;
the preparation method of the graphite oxide phase carbon nitride is characterized by comprising the following steps:
s1: adding 4×10 in mass fraction into a reaction vessel 4 -9×10 4 Mixing the acid solution, and cooling to below 10 ℃; then adding 1×10 respectively 3 -1.5×10 3 Part graphite phase carbon nitride and 0.5 x 10 3 -1.5×10 3 The oxidation promoter is added and fully stirred to be uniformly dispersed; finally, adding 1-5 parts of oxidation stabilizer, and fully stirring to uniformly disperse the oxidation stabilizer to obtain solution A;
s2: maintaining the temperature below 10 ℃ and adding 3X 10 to the solution A by mass fraction 3 -5×10 3 Potassium ferrate is added and fully stirred for 1.5-2h; heating to 25-35deg.C, adding 2×10 3 -4×10 3 Potassium ferrate is added and fully stirred for 2-3h; finally, heating to 45-50 ℃ and stirring for 1.5-2h to obtain a solution B;
s3: centrifuging the solution B obtained in the step S2, standing to obtain supernatant and precipitate, and washing the precipitate with pure water; repeating the centrifugation, standing and washing processes until the pH value of the supernatant is 6.5-7.5, and obtaining the final precipitate;
s4: freeze-drying the final precipitate obtained in the step S3 by a vacuum freeze dryer to obtain graphite oxide phase carbon nitride;
in the S1, the mixed acid liquid is a mixed solution of sulfuric acid and hydrochloric acid, wherein the mass ratio of the sulfuric acid to the hydrochloric acid is 30:1-70:1;
in S1, the oxidation stabilizer is at least one of periodic acid and citric acid;
in S1, the oxidation promoter is at least one of sodium nitrate and potassium nitrate.
2. The use according to claim 1, wherein in S1 the oxidation stabilizer is a mixture of periodic acid and citric acid, wherein the mass ratio of periodic acid to citric acid is 1:2-2:1.
3. The use according to claim 1, wherein the graphite oxide phase carbon nitride is used for the loading of silver nanoparticles.
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| Environmentally Sustainable Fabrication of Ag@g-C3N4 Nanostructures and Their Multifunctional Efficacy as Antibacterial Agents and Photocatalysts;Mohammad Ehtisham Khan, et al;《ACS Applied Nano Materials》;第1卷(第6期);第2912-2922页 * |
| 多孔石墨相氮化碳限域Ag/Au纳米颗粒催化还原对硝基苯酚;田逢雨;胡付超;侯东芳;乔秀清;李东升;;中国科学:化学(06);全文 * |
| 玉米淀粉高锰酸钾氧化法的探讨──玉米淀粉氧化方法及高效催化剂表征研究;王彦斌，苏琼;西北民族学院学报(自然科学版)(02);全文 * |
| 生物质石墨烯/LaFeO_3纳米复合材料的光催化活性;矫立志;张京茹;董抒华;王靖朝;谷国华;陈川东;魏春城;;人工晶体学报(01);全文 * |
| 用于空气净化领域的石墨相氮化碳宏观光催化剂的研究;阳叶;《中国优秀硕士学位论文全文数据库 工程科技I辑》(第7期);第14页章节2.2.2 * |
| 阳叶.用于空气净化领域的石墨相氮化碳宏观光催化剂的研究.《中国优秀硕士学位论文全文数据库 工程科技I辑》.2019,(第7期),第14页章节2.2.2. * |
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