CN112010272B - Delaminated carbon nitride material and preparation method thereof - Google Patents

Delaminated carbon nitride material and preparation method thereof Download PDF

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CN112010272B
CN112010272B CN201910468081.0A CN201910468081A CN112010272B CN 112010272 B CN112010272 B CN 112010272B CN 201910468081 A CN201910468081 A CN 201910468081A CN 112010272 B CN112010272 B CN 112010272B
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specific surface
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formic acid
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王峰
苏凯艺
张超锋
高著衍
任濮宁
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Dalian Institute of Chemical Physics of CAS
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    • 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
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    • B82Y40/00—Manufacture or treatment of nanostructures
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    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

Abstract

The invention relates to a preparation method of a delaminated carbon nitride nano flaky material. G to C3N4Dispersing in formic acid solvent, putting in light-permeable synthesis kettle, sealing, keeping out of the sun, and introducing O2Stirring for 1-60 h at 20-40 ℃, and then exposing to illumination of 250-780 nm for 1-180 h. And after the reaction is finished, separating, washing and drying the precipitate to obtain the carbon nitride nanosheet-shaped material with the layer stripped. The specific surface area of the material is 18-313 m2Between/g, the material is of a layered structure and has potential application in the fields of catalysis, organic photoelectric conversion, sensors and the like.

Description

Delaminated carbon nitride material and preparation method thereof
Technical Field
The invention belongs to the technical field of material synthesis, and particularly relates to a preparation method of a delaminated carbon nitride nano flaky material.
Background
Carbon and nitrogen elements widely exist in nature, and carbon nitride materials have important application in catalysis, electrodes, sensors and lithium battery electrode materials. A common compound for carbon nitride materials is carbon nitride (g-C) in the graphite phase3N4) Of real g-C3N4Is a very complex system with the element composition removedCarbon and nitrogen elements are present, as well as many hydrogen or oxygen elements. Compared with the prior art, the specific surface area is lower (< 10 m)2G), larger block g-C3N4In some cases differently element doped or structurally modulated g-C3N4Can show more excellent performance in the photocatalytic selective oxidation reaction.
At present, from block g-C3N4Starting from the preparation of lamellar Nanog-C3N4The synthesis of the material has the following aspects: zhang et al (chem. Commun.,2017,53,9430-9433.) use solid phase high temperature synthesis by further calcining the lumpy g-C3N4Obtaining flakes g-C of high specific surface3N4A material. The method needs to undergo high-temperature solid-phase reaction during synthesis. S. Kang et al (Green chem.,2018,20,1354-1361.) by using g-C in block form3N4Introducing NaClO for long-time high-temperature crystallization treatment to obtain g-C with sheet-shaped high specific surface3N4A material. Wherein the strong oxidizing power of NaClO is utilized to oxidize nitrogen atoms on the carbon nitride skeleton, and the block-shaped g-C3N4The material is stripped. Mu et al (Green chem.,2017,19,5041-5045.) use and bulk g-C3N4The gamma-valerolactone with the specific surface energy close to that of the gamma-valerolactone is subjected to long-time ultrasonic treatment to obtain flaky g-C with high specific surface3N4A material. Similar to the long-time ultrasonic method, a preparation method using a strong acid or a mixed acid as a solvent (Appli. Catal. B: environ.2017,217, 629-636) is also provided.
Relevant studies have found flaky or delaminated g-C3N4The method has good advantages in the photocatalytic selective oxidation reaction, but the synthesis method is mostly a solid-phase high-temperature reaction, or partial oxidation reduction at high-temperature hydrothermal or long-time ultrasonic treatment by using strong acid and alcohol, the yield is low or the ultrasonic time is long, and the energy consumed in the synthesis process is huge, so that the development of green delaminated g-C is urgently needed3N4The preparation method of (1). According to the previous literature reports (Angew. chem. int. Ed.2017,27,3992-To utilize the g-C of the gas generated in the reaction relative to the phase3N4And (5) realizing stripping. And may be in the form of chunks g-C in the presence of a reducing or oxidizing agent3N4Manufacturing vacant sites, destroying the repeated structure among layers and realizing layer stripping.
The material structure determines the performance of the material, so that the development of a reliable and structurally controllable synthesis method of the carbon nitride nano flaky material has important significance. The carbon nitride nano sheet material prepared by the photo-assisted method has potential application in the fields of catalysis, organic photoelectric materials, sensors and the like because of the unique structure.
Disclosure of Invention
The invention provides a method for preparing carbon nitride nano flaky material by illumination-assisted stripping, which utilizes illumination to contain blocky g-C on the basis of carbon nitride3N4The obtained formic acid solution has good thermal stability and large specific surface area (18-300 m)2G) flakes of g-C3N4It is suitable for catalysis, organic photoelectric material, sensor and other fields.
The technical scheme of the invention is as follows: will contain g-C3N4The compound is dispersed in formic acid solution, placed in a light-permeable synthesis kettle, sealed and then introduced with 0.1-10 MPa of O2And (3) keeping out of the sun, stirring for 1-60 h at 20-40 ℃, and then exposing to light of 250-780 nm for 1-180 h. And after the reaction is finished, separating, washing and drying the precipitate to obtain the carbon nitride nano flaky material.
The carbon nitride material is different from a thermal or ultrasonic method reported in the literature in a delamination method, and the delamination degree can be controlled by the illumination time. The preparation principle of the material is as follows: the size of the formic acid molecule is calculated to be 0.31nm, and the surface energy is calculated to be 65.8mJ/m2With block g-C3N4Surface energy is close to (-70 mJ/m)2) And formic acid can generate CO under illumination2Thus, CO decomposed by formic acid under illumination can be utilized2For stripping, wherein formic acid is used as a reducing agent for g-C in addition to a gas source3N4The upper N atom is reduced. Thus the process herein proposes a method of photo-assisted delamination to produce a sheet-like g-C3N4A material.
The concentration of the formic acid solution has an important influence on the synthetic material. Formic acid with different concentrations has different improved reduction degrees and different bubble amounts, and the concentration of a suitable formic acid solution is as follows: 0.0001-10.0 mol/L, preferably the concentration of the formic acid solution is as follows: 0.001-5.0 mol/L, and the optimal concentration of the formic acid solution is as follows: 0.2 to 1.0 mol/L. Suitable amounts of formic acid solution are: 0.05-0.5 mL (formic acid solution)/mg (g-C)3N4) The preferred amount of formic acid solution is: 0.1-0.3 mL (formic acid solution)/mg (g-C)3N4) The optimal amount of the formic acid solution is as follows: 0.2-0.25 mL (formic acid solution)/mg (g-C)3N4)。
Besides selecting the concentration of the formic acid solution which is properly matched, the key point of the material synthesis lies in reasonably adjusting the stirring temperature, the concentration of the mother solution and O2Pressure, exposure reaction time, exposure wavelength, and the like. The suitable dispersion temperature is 20 ℃ to 40 ℃, the preferred mixing temperature is 30 ℃ to 40 ℃, and the most preferred mixing temperature is 30 ℃ to 35 ℃.
Suitable concentrations for solution a are: 0.008-1.0 mol/L, and the preferable concentration of the solution A is as follows: 0.01-0.5 mol/L, and the optimal concentration of the solution A is as follows: 0.02-0.1 mol/L. Suitable stirring times in the dark are: 1-60 h, and the preferable light-resistant stirring time is as follows: 10-45 h, and the optimal light-resistant stirring time is as follows: 20-30 h. Suitable exposure reaction times are: 1-180 h, and the preferable reaction time is as follows: 24-144 h, and the optimal reaction time is as follows: 72-96 h. Suitable wavelengths of illumination are: 250-780 nm, and the preferable illumination wavelength is as follows: 320-780 nm, and the optimal illumination wavelength is as follows: 400 to 780 nm. Suitable O2Pressure: 0.1 to 5MPa, preferably O2The pressure is as follows: 0.5 to 5MPa, preferably O2The pressure is as follows: 1.0 to 2.0 MPa.
The invention relates to a preparation method of a carbon nitride nano sheet material, which has the advantages that:
(1) the synthesized material is processed by illumination on the basis of carbon nitride, which is different from high-temperature heat treatment and ultrasonic treatment,provides a green preparation method, and the specific surface area of the preparation method is 18-313 m2Between/g, a material having a layered structure on the crystal structure.
(2) The preparation method is simple and easy to control synthesis. The obtained material can be used in the fields of catalysis, organic photoelectric conversion, sensors and the like.
Drawings
FIG. 1 is a transmission electron micrograph of a delaminated carbon nitride nanosheet material prepared in example 1.
FIG. 2 shows g-C3N4And the activity of the carbon nitride nanosheet material prepared in example 14 in photocatalytic benzyl alcohol oxidation.
Reaction conditions are as follows: 10mg of catalyst, 1mL of a 0.1mmol solution of benzyl alcohol in acetonitrile, O2(1atm), reaction time 8h, reaction temperature 40 ℃, light wavelength 455nm, 6W LEDs.
The specific implementation mode is as follows:
in order to further explain the present invention in detail, several specific embodiments are given below, but the present invention is not limited to these embodiments.
Example 1:
0.1g of g-C3N4Dispersing in 5mL of 0.0001mol/L formic acid solution, placing in a light-permeable synthesis kettle with initial temperature of 20 deg.C, introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 18m2/g。
Example 2:
0.1g of g-C3N4Dispersing in 10mL of 0.001mol/L formic acid solution, and addingIntroducing 5MPa of O into a light-permeable synthesis kettle with the initial temperature of 20 DEG C2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 23m2/g。
Example 3:
0.1g of g-C3N4Dispersing in 20mL of 0.2mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 95m2/g。
Example 4:
0.1g of g-C3N4Dispersing in 25mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Using Micromeritics ASDetermining specific surface area of sample by AP 2010 physical adsorption instrument, vacuum treating the sample at 120 deg.C for more than 3 hr to make vacuum degree reach 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 103m2/g。
Example 5:
0.1g of g-C3N4Dispersing in 30mL of 5.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 81m2/g。
Example 6:
0.1g of g-C3N4Dispersing in 50mL of 10mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 56m2/g。
Example 7:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 136m2/g。
Example 8:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 175m2/g。
Example 9:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nanosheet is obtained through centrifugal separation, deionized water washing and vacuum dryingAs a material. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 163m2/g。
Example 10:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 148m2/g。
Example 11:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Adsorption of nitrogenThe desorption experiment shows that the specific surface of the material is 99m2/g。
Example 12:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 189m2/g。
Example 13:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 2MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 213m2/g。
Example 14:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 1MPa of O2Stirring for 60h in the dark, and then exposing to light of 250-780 nmAnd (5) irradiating for 180 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 221m2/g。
Example 15:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 0.5MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 192m2/g。
Example 16:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 20 ℃, and introducing 0.1MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degreeTo 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 167m2/g。
Example 17:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 30 ℃, and introducing 2.0MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 225m2/g。
Example 18:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 234m2/g。
Example 19:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, and addingIntroducing 2.0MPa of O into a light-permeable synthesis kettle with the initial temperature of 40 DEG C2And stirring for 60 hours in the dark, and then exposing the mixture to the illumination of 250-780 nm for 180 hours. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 180m2/g。
Example 20:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 45h in the dark, and then exposing to the illumination of 250-780 nm for 180 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 248m2/g。
Example 21:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 30h in the dark, and then exposing to the illumination of 250-780 nm for 180 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Using MicMeasuring the specific surface area of the sample by a romeritics ASAP 2010 physical adsorption instrument, and before the measurement, carrying out vacuum treatment on the sample at 120 ℃ for more than 3h to ensure that the vacuum degree reaches 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 265m2/g。
Example 22:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 20h in the dark, and then exposing to the illumination of 250-780 nm for 180 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 258m2/g。
Example 23:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 10h in the dark, and then exposing to the illumination of 250-780 nm for 180 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 243m2/g。
Example 24:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 1h in the dark, and then exposing to the illumination of 250-780 nm for 180 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 233m2/g。
Example 25:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 30h in the dark, and then exposing to light of 320-780 nm for 180 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 277m2/g。
Example 26:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 30h in the dark, and then exposing to the light of 400-780 nm for 180 h. After the synthesis is finished, centrifugal separation is carried out, and deionized water washing vacuum is carried outDrying to obtain the carbon nitride nano flaky material. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 285m2/g。
Example 27:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 30h in the dark, and then exposing to the light of 400-780 nm for 144 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10-6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 287m2/g。
Example 28:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 30h in the dark, and then exposing to the light of 400-780 nm for 96 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10- 6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), the ratioThe surface area is calculated using the BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 313m2/g。
Example 29:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 30h in the dark, and then exposing to the light of 400-780 nm for 72 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10- 6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 302m2/g。
Example 30:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPa of O2And stirring for 30h in the dark, and then exposing to the light of 400-780 nm for 24 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10- 6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 291m2/g。
Example 31:
0.1g of g-C3N4Dispersing in 20mL of 1.0mol/L formic acid solution, placing in a light-permeable synthesis kettle with an initial temperature of 35 ℃, and introducing 2.0MPO of a2And stirring for 30h in the dark, and then exposing to the light of 400-780 nm for 1 h. After the synthesis is finished, the carbon nitride nano flaky material is obtained by centrifugal separation, deionized water washing and vacuum drying. And (3) observing the prepared carbon nitride material to be in a sheet structure by using a transmission electron microscope test. Measuring specific surface area of sample with Micromeritics ASAP 2010 physical adsorption instrument, and vacuum treating the sample at 120 deg.C for more than 3 hr to reach vacuum degree of 10- 6About torr, and then the test is carried out at the liquid nitrogen temperature (-196 ℃), and the specific surface area is calculated by adopting a BET equation. Nitrogen adsorption and desorption experiments show that the specific surface of the material is 21m2/g。

Claims (4)

1. A preparation method of a delaminated carbon nitride nano flaky material is characterized by comprising the following steps:
g to C3N4Dispersing in formic acid solution, putting in a light-transmitting synthesis kettle, and introducing 0.1-5 MPa of O2Is sealed and light-proof at 20-40 deg.CoStirring for 1-60 h under C, then exposing to illumination of 250-780 nm for 1-180 h, after the reaction is finished, performing centrifugal separation on the precipitate, washing with deionized water, and drying to obtain a carbon nitride nanosheet-shaped material with a layer removed;
the amount of formic acid used is: 0.2-0.5 mL (formic acid solution)/mg (g-C)3N4) The concentration of the formic acid solution is: 0.2 to 10 mol/L.
2. The method of claim 1, wherein:
the stirring temperature is 30-35 ℃ in the darkoAnd C, stirring for 20-30 h.
3. The method of claim 1, wherein:
the wavelength of the illumination is as follows: 400-780 nm; the illumination time is as follows: 72-96 h.
4. The method of claim 1, wherein:
transparent photosynthesisIntroducing O into the finished kettle2The pressure of (A) is: 1 to 2 MPa.
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