CN107954405A - g-C3N4The preparation method of colloidal sol - Google Patents
g-C3N4The preparation method of colloidal sol Download PDFInfo
- Publication number
- CN107954405A CN107954405A CN201711174318.1A CN201711174318A CN107954405A CN 107954405 A CN107954405 A CN 107954405A CN 201711174318 A CN201711174318 A CN 201711174318A CN 107954405 A CN107954405 A CN 107954405A
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- China
- Prior art keywords
- water
- aqueous solution
- coupling agent
- silane coupling
- particle
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
- B01J13/0026—Preparation of sols containing a liquid organic phase
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The present invention relates to field of semiconductor materials, it is desirable to provide a kind of g C3N4The preparation method of colloidal sol.Including：Rich nitrogen presoma is heat-treated, is cooled to room temperature rear ball milling, obtains g C3N4Particle；By g C3N4Particle is scattered in acidic aqueous solution, and mixed liquor is obtained after supersonic oscillations under condition of water bath heating；Mixed liquor is added in silane coupling agent aqueous solution by the speed of 2ml/min, 6h is stood after adding；After the precipitation filtering of acquisition, washing, it is scattered in water-alcohol solvent, obtains g C3N4Colloidal sol.The present invention is by improving g C3N4The dispersion stabilization of nano particle, obtains g C3N4Colloidal sol, avoids the reunion of nano particle during light-catalyzed reaction.Solve g C3N4Be not easy the problem of compound with other materials, etched by strong acid, surface in situ be modified etc. means add g C3N4Surface reaction activity site, is conducive to g C3N4Nano particle and other materials it is compound, be g C3N4The research of based nano composite material provides new thinking.
Description
Technical field
The present invention is on field of semiconductor materials, more particularly to a kind of g-C3N4The preparation method of colloidal sol.
Background technology
Since energy problem and environmental problem become all the more serious, photocatalysis technology has become most promising at present
One of science and technology.And class graphitic nitralloy carbon (g-C3N4) because of its special physical and chemical performance, protected in Solar use, environment
The fields such as shield show good application prospect, have caused extensive concern.However, bulk g-C3N4Due to high electron-hole pair
Compound probability, relatively low quantum efficiency, less absorption site and avtive spot, cause its photocatalysis efficiency poor, limit
Its extensive use.
There are many methods to improve g-C at present3N4Catalytic efficiency, such as bulk g-C3N4The control of configuration of surface, system
It is standby go out new nanostructured, utilize foreign atom to be modified etc..At present in nanostructured control aspect, study in g-C3N4
Quantum dot, nanometer rods, nanometer sheet, mesoporous block materials etc. achieve impressive progress.Experiment proves there is certain nano junction
The g-C of structure3N4Specific surface area can effectively be increased, promote photo-generate electron-hole to improve composite material quantum efficiency, performance to separation
Outstanding photocatalysis performance.But, current g-C3N4Nanometer rods, nanometer sheet still suffer from agglomeration in use,
Reduce photocatalysis efficiency；And g-C3N4Though quantum dot can be preferably scattered in liquid phase, due to there are quantum confined effect, its
Photocatalytic activity is relatively low.Therefore, g-C is solved3N4The dispersiveness of nano material is of great significance its photocatalytic applications.
The content of the invention
The technical problem to be solved in the present invention is overcome g-C in the prior art3N4The difficult scattered deficiency of nano material, there is provided
A kind of g-C3N4The preparation method of colloidal sol.
In order to solve the above technical problems, the solution of the present invention is：
A kind of g-C is provided3N4The preparation method of colloidal sol, includes the following steps：
Step A：A certain amount of rich nitrogen presoma is placed in corundum boat, is heat-treated in tube furnace；Natural cooling
To room temperature, by product ball milling, g-C is obtained3N4Particle；
The heat treatment temperature is 450~600 DEG C；Heating rate is 1.5~4 DEG C/min；Soaking time is 2~6h；Ball
The process conditions of mill are：Ratio of grinding media to material 20:1~40:1,200~500r/min of ball milling speed, 2~12h of Ball-milling Time.
Step B：By g-C3N4Particle is scattered in acidic aqueous solution, is obtained after supersonic oscillations under condition of water bath heating
Mixed liquor；Mixed liquor is added in silane coupling agent aqueous solution by the speed of 2ml/min, 6h is stood after adding；By the heavy of acquisition
Form sediment after filtering, washing, be scattered in water-alcohol solvent, obtain g-C3N4Colloidal sol；
Wherein, the concentrated nitric acid that the concentrated sulfuric acid that it is 98% by mass fraction that acidic aqueous solution, which is, is 68% with mass fraction is prepared
Form, the mass ratio of the concentrated sulfuric acid and concentrated nitric acid is 1:2~2:1；g-C3N4The mass ratio of particle and acidic aqueous solution is 1:50~1:
200；Bath temperature is 50~80 DEG C, ultrasonic frequency 40kHz, and the supersonic oscillations time is 1~4h；Silane coupling agent is water-soluble
Silane coupling agent and the mass ratio of deionized water are 1 in liquid:100~1:1000, the matter of mixed liquor and silane coupling agent aqueous solution
Amount is than being 1:10~1:20；Water-alcohol solvent is by deionized water and absolute ethyl alcohol in mass ratio 10:1~1:4 are formulated, precipitation
Mass ratio with water-alcohol solvent is 1:50~1:200.
In the present invention, rich nitrogen presoma described in step A is one or two and thiocarbamide, the urea of cyanamide, dicyandiamide
One or both of combination.
In the present invention, silane coupling agent described in step B for gamma-aminopropyl-triethoxy-silane, N- (β-aminoethyl)-
The basic silane coupling agents such as γ-aminopropyltrimethoxysilane, N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane
At least one of.
In the present invention, in the step B, before using water-alcohol solvent, by adding hydrochloric acid or ammonium hydroxide by water-alcohol solvent
PH value be adjusted to 5~9.
The realization principle of the present invention：
(1) using the rich nitrogen presoma of compounding, the ammonia produced by the use of thiocarbamide, urea is prepared as template has loose knot
The g-C of structure3N4Particle, is conducive to follow-up g-C3N4The stripping refinement of particle；(2) loose g- is peeled off using composite strong acid etching
C3N4Particle, makes g-C3N4Particle surface, inside are almost peeled off at the same time, are conducive to obtain the homogeneous g-C of shape size3N4Nanometer
Grain；(3) it is modified to form steric hindrance raising g-C using silane coupling agent in-situ hydrolysis3N4The dispersion stabilization of nano particle, is obtained
Obtain g-C3N4Colloidal sol, and nanoparticle surface charge state is changed by adjustment and control system pH value, further improve Stability of Sols
Property.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, the present invention is by improving g-C3N4The dispersion stabilization of nano particle, obtains g-C3N4Colloidal sol, avoids photocatalysis
The reunion of nano particle in reaction process.
2nd, the present invention solves g-C3N4The problem of compound is not easy with other materials, is etched by strong acid, surface in situ is modified
G-C is added etc. means3N4Surface reaction activity site, is conducive to g-C3N4Nano particle and other materials it is compound, be g-
C3N4The research of based nano composite material provides new thinking.
Brief description of the drawings
Fig. 1 is g-C3N4The dried stereoscan photograph of colloidal sol (apparent form photo).
Embodiment
The present invention is described in further detail with reference to embodiment：
g-C3N4The preparation method of colloidal sol, includes the following steps：
Step A：A certain amount of rich nitrogen presoma is placed in corundum boat, is heat-treated in tube furnace.Then it is natural
It is cooled to room temperature, product ball milling is obtained into loose g-C3N4Particle.
Wherein, heat treatment temperature is 450~600 DEG C；Heating rate is 1.5~4 DEG C/min；Soaking time is 2~6h.Ball
Grinding process condition is：Ratio of grinding media to material 20:1~40:1,200~500r/min of ball milling speed, 2~12h of Ball-milling Time.
Step B：By obtained g-C3N4Particle is scattered in acidic aqueous solution, then surpasses it under condition of water bath heating
Sonication obtains mixed liquor afterwards for a period of time；Then mixed liquor is slowly added to silane coupling agent water by the speed of 2ml/min
In solution, mixed liquor stands 6h after being added completely into, and the precipitation of acquisition is filtered, is washed, and is then dispersed in a certain amount of water
In alcoholic solvent, g-C is obtained3N4Colloidal sol.
Wherein, the concentrated nitric acid that acidic aqueous solution is 98% by mass fraction the concentrated sulfuric acid is 68% with mass fraction prepare and
Into the mass ratio of the concentrated sulfuric acid and concentrated nitric acid is 1:2~2:1；g-C3N4The mass ratio of particle and acidic aqueous solution is 1:50~1:
200；Bath temperature is 50~80 DEG C, ultrasonic frequency 40kHz, and the supersonic oscillations time is 1~4h；Silane coupling agent is water-soluble
Silane coupling agent and the mass ratio of deionized water are 1 in liquid:100~1:1000, the matter of mixed liquor and silane coupling agent aqueous solution
Amount is than being 1:10~1:20；Water-alcohol solvent is by deionized water and absolute ethyl alcohol in mass ratio 10:1~1:4 are formulated, white
The mass ratio of precipitation and water-alcohol solvent is 1:50~1:200.
The present invention is more fully understood in the professional technician that the following examples can make this professional, but not with any side
The formula limitation present invention.G-C is successfully made by 9 embodiments respectively3N4Colloidal sol, the test data in each embodiment see the table below 1.
1 embodiment tables of data of table
Finally, it should also be noted that it is listed above be only the present invention specific embodiment.Obviously, the present invention not
It is limited to above embodiment, there can also be many deformations.Those of ordinary skill in the art can be straight from present disclosure
Export or all deformations associated are connect, are considered as protection scope of the present invention.
Claims (4)
- A kind of 1. g-C3N4The preparation method of colloidal sol, it is characterised in that include the following steps：Step A：A certain amount of rich nitrogen presoma is placed in corundum boat, is heat-treated in tube furnace；Naturally cool to room Wen Hou, by product ball milling, obtains g-C3N4Particle；The heat treatment temperature is 450~600 DEG C；Heating rate is 1.5~4 DEG C/min；Soaking time is 2~6h；Ball milling Process conditions are：Ratio of grinding media to material 20:1~40:1,200~500r/min of ball milling speed, 2~12h of Ball-milling Time；Step B：By g-C3N4Particle is scattered in acidic aqueous solution, is mixed after supersonic oscillations under condition of water bath heating Liquid；Mixed liquor is added in silane coupling agent aqueous solution by the speed of 2ml/min, 6h is stood after adding；By the precipitation of acquisition After filter, washing, it is scattered in water-alcohol solvent, obtains g-C3N4Colloidal sol；Wherein, the concentrated nitric acid that it is 98% by mass fraction that acidic aqueous solution, which is, the concentrated sulfuric acid is 68% with mass fraction prepare and Into the mass ratio of the concentrated sulfuric acid and concentrated nitric acid is 1:2~2:1；g-C3N4The mass ratio of particle and acidic aqueous solution is 1:50~1: 200；Bath temperature is 50~80 DEG C, ultrasonic frequency 40kHz, and the supersonic oscillations time is 1~4h；Silane coupling agent is water-soluble Silane coupling agent and the mass ratio of deionized water are 1 in liquid:100~1:1000, the matter of mixed liquor and silane coupling agent aqueous solution Amount is than being 1:10~1:20；Water-alcohol solvent is by deionized water and absolute ethyl alcohol in mass ratio 10:1~1:4 are formulated, precipitation Mass ratio with water-alcohol solvent is 1:50~1:200.
- 2. according to the method described in claim 1, it is characterized in that, rich nitrogen presoma is cyanamide, dicyandiamide described in step A One or two and the combination of one or both of thiocarbamide, urea.
- 3. according to the method described in claim 1, it is characterized in that, silane coupling agent described in step B is three second of γ-aminopropyl Oxysilane, N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxy At least one of basic silane coupling agent such as base silane.
- 4. according to the method described in claim 1, it is characterized in that, in the step B, before using water-alcohol solvent, pass through The pH value of water-alcohol solvent is adjusted to 5~9 by addition hydrochloric acid or ammonium hydroxide.
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| CN201711174318.1A CN107954405A (en) | 2017-11-22 | 2017-11-22 | g-C3N4The preparation method of colloidal sol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109279585A (en) * | 2018-09-30 | 2019-01-29 | 北华大学 | A kind of nonmetallic g-C3N4The preparation method of nanometer sheet |
| CN115873482A (en) * | 2022-12-12 | 2023-03-31 | 湖北大学 | Polyurea elastomer composite coating material, preparation method and application thereof |
| CN116948449A (en) * | 2023-07-28 | 2023-10-27 | 浙江大学 | Preparation method of special composite sol for neodymium-iron-boron magnet |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103170358A (en) * | 2013-04-08 | 2013-06-26 | 清华大学 | Porous g-C3N4 photocatalyst and preparation method thereof |
| CN104017313A (en) * | 2014-03-14 | 2014-09-03 | 江苏大学 | Graphite-like carbon nitride/polyvinylidene fluoride composite material and preparation method thereof |
| CN106379874A (en) * | 2016-09-27 | 2017-02-08 | 浙江大学 | Preparation method of g-C3N4 nanosphere |
-
2017
- 2017-11-22 CN CN201711174318.1A patent/CN107954405A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103170358A (en) * | 2013-04-08 | 2013-06-26 | 清华大学 | Porous g-C3N4 photocatalyst and preparation method thereof |
| CN104017313A (en) * | 2014-03-14 | 2014-09-03 | 江苏大学 | Graphite-like carbon nitride/polyvinylidene fluoride composite material and preparation method thereof |
| CN106379874A (en) * | 2016-09-27 | 2017-02-08 | 浙江大学 | Preparation method of g-C3N4 nanosphere |
Non-Patent Citations (1)
| Title |
|---|
| QIFENG CAI ET AL.: "Template-free preparation and characterization of nanoporous g-C3N4 with enhanced visible photocatalytic activity", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109279585A (en) * | 2018-09-30 | 2019-01-29 | 北华大学 | A kind of nonmetallic g-C3N4The preparation method of nanometer sheet |
| CN115873482A (en) * | 2022-12-12 | 2023-03-31 | 湖北大学 | Polyurea elastomer composite coating material, preparation method and application thereof |
| CN115873482B (en) * | 2022-12-12 | 2023-11-14 | 湖北大学 | Polyurea elastomer composite coating material, preparation method and application thereof |
| CN116948449A (en) * | 2023-07-28 | 2023-10-27 | 浙江大学 | Preparation method of special composite sol for neodymium-iron-boron magnet |
| CN116948449B (en) * | 2023-07-28 | 2024-04-02 | 浙江大学 | Preparation method of special composite sol for neodymium-iron-boron magnet |
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Application publication date: 20180424 |
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