CN109292752A - A kind of preparation method of the meso-porous carbon material of phosphorus doping functionalization - Google Patents
A kind of preparation method of the meso-porous carbon material of phosphorus doping functionalization Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of the meso-porous carbon material of phosphorus doping functionalization, comprise the following steps: (1) preparation of mixed liquor A；(2) preparation of mixed liquid B；(3) preparation of phosphorous composite precursor；(4) carbonization treatment of phosphorous composite precursor；(5) preparation of sample MC-TPP；The present invention is fused together both functional element doping and mesoporous synthesis novelty, realize synchronous preparation, different phosphorus sources is investigated, optimal with the effect of triphenyl phosphorus, triphenyl phosphorus is as important presoma, it is not only the doping offer phosphorus source of carbon, and the additive of mesoporous synthesis is served as, play the role of reaming, prepared material has uniform meso-hole structure, the advantages that phosphorus doping effect is excellent, element good dispersion.
Description
Technical field
The present invention relates to technical field of inorganic material, and in particular to a kind of preparation of the meso-porous carbon material of phosphorus doping functionalization
Method.
Background technique
It is well known that (such as adsorbing) many performances of carbon material in actual use are often depending on the pore structure of material
With Surface Physical Chemistry characteristic, not only the surface of the physical parameters impacts carbon material such as the aperture of material, Kong Rong and specific surface area is inhaled
It is attached, and the chemical characteristic of carbon material surface also plays the part of important angle in specific absorption, catalyst load and surface reaction
Color, due to the chemical inertness and stability of carbon material, so that its functionalization is difficult compared with silicon-based mesoporous material, therefore carbon material surface
The research of functionalization becomes meaningful and rich in challenge.The functionalization of carbon material surface includes oxygen, nitrogen, phosphorus, boron, chlorine, fluorine
Etc. heteroatomic doping.Oxygen-containing functional group can make carbon-based material have better hydrophily and cation exchange capacity (CEC), together
When also help modification load other noble metals.The generation of the oxygen-containing functional group of carbon material surface generally uses HNO3 to aoxidize
The method of post-processing, make its surface oxygen groups increase, in this way can with the subsequent further functionalization of carried noble metal particle, but its
Middle shortcoming is the reduction collapsed with the degree of order that easy post-processing leads to carbon material part hole, therefore direct synthesized element
Doped carbon material functional just becomes preferred method, and this method generally selects itself containing miscellaneous when selecting carbon matrix precursor
The compound of atom is as precursor.For example the synthesis of nitrogen-doped carbon can choose the carbon source containing nitrogen-atoms such as polyacrylonitrile, pyrrole
It coughs up, one or more steps synthesis is handled by high temperature cabonization and realizes N doping.The result of study of nitrogen-doped carbon material shows its tool
Have good physical property and chemical property, this show Heteroatom doping will affect the acid-base property of carbon material to modulation they
Electrochemical properties and catalytic performance.Some results of study show that the carbon material of P elements doping equally has many special property
Matter, these properties include acidic functionality, ion-exchange capacity and enhancing oxidability.Wan passes through research phosphorus doping diamond-like
Stone carbon film, discovery phosphorus doping carbon can increase current density in high electric field, and the excellent field emission performance of this doping membrane material is main
Because material surface pattern and due to doping cause the change of material microstructure to influence.Puziy etc. is with phosphoric acid and styrene-diethyl
Alkenyl benzene polymer is that source roasts synthesis carbon material at different temperatures, and obtained carbon material possesses acid and is similar at oxidation
The ion-exchange capacity of carbon is managed, this acid carbon material handled with phosphoric acid is more stable relative to the carbon material of oxidation processes.So
They have selected phosphoric acid and three kinds of carbon sources (drupe, styrene-diethylbenzene, bismelimidodiphenylmethane- again afterwards
Divinylbenzene copolymer) in 800 DEG C of roastings obtain the micro-pore carbon material containing phosphorus functionalization.The result of electrochemical analysis
Illustrate that the material can greatly enhance the energy force density of supercapacitor.A large amount of works have been done in terms of phosphorus doping by Puziy seminar
Make, they obtain the carbon material of phosphoric acid functionalized by high-temperature roasting based on different carbon sources and phosphoric acid mixing, and this method is not
The porous of carbon material can only be improved and a large amount of phosphorus can be wrapped up inside carbon material.
A kind of phosphorus doping micropore/meso-porous carbon material and its preparation side are disclosed in Chinese patent CN108609604A at present
Method belongs to preparation and the applied technical field of carbon material.It is to be dried after cleaning up gumbo with clear water, -45 DEG C~-80 DEG C items
It is lyophilized 48 hours~96 hours under part, obtains freeze-drying gumbo；It is heat-treated 2 hours~4 hours under the conditions of 700 DEG C~900 DEG C again,
Obtain phosphorus doping micropore/meso-porous carbon material.Prepared phosphorus doping micropore/meso-porous carbon material is three-dimensional porous structure, micropore hole
Having a size of 0.5~1.8nm, micropore pore volume is 0.3~0.8cm3/g, and mesoporous pore size is 5~10nm, pore volume is 0.8~
1.5cm3/g, BET specific surface area are 600~900m2/g, and the doping content of phosphorus atoms is 4~12wt%.Prepared phosphorus doping
Micropore/meso-porous carbon material have big specific surface area, big porosity and regulatable pore-size distribution, while also have micropore and
The hole of mesoporous two kinds of sizes, these unique porous structures have phosphorus doping micropore/meso-porous carbon material emphatically in many fields
The application prospect wanted.
But existing meso-porous carbon material usually has that phosphorus doping effect is poor, the defect of element bad dispersibility.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of systems of the meso-porous carbon material of phosphorus doping functionalization
Preparation Method effectively compensates for defect of the existing technology.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of preparation method of the meso-porous carbon material of phosphorus doping functionalization, comprises the following steps:
(1) 1.5-3g triblock copolymer is dissolved in 30-75ml distilled water first, 2-7.5g sucrose is added, is sufficiently stirred
Dissolution, then adds appropriate triphenyl phosphorus and 15-30ml ethyl alcohol thereto, is stirred at room temperature uniformly, 3.4-6.9mL then is being added just
Mixed liquor A is sufficiently stirred to obtain in silester；
(2) mixed liquor A is moved into single-necked flask, is stirred under 40 DEG C of water baths, with 0.5ml/min in whipping process
The hydrochloric acid solution of a certain amount of 2mol/L is added dropwise, is stirred overnight under the water bath, obtains mixed liquid B；
(3) mixed liquid B is moved into autoclave, hydro-thermal reaction certain time takes lower layer after the reaction was completed under the conditions of 373K
Product, it is dry under the conditions of 353K, obtain phosphorous composite precursor；
(4) by phosphorous composite precursor in high temperature Muffle furnace, carbonization treatment 2h under conditions of 574K, then by temperature
It is warming up to 1173K with the speed of 10K/min, keeps 3h；
(5) under the conditions of 373K, step (4) products therefrom is refluxed overnight with the ethanol water containing sodium hydroxide, is gone
Except silica, then continue the 12h that flows back with distilled water, finally moves to vacuum to the aobvious neutrality of solution with distilled water eccentric cleaning
Drying box is dry, and sample is denoted as MC-TPP.
Preferably, the additive amount of triphenyl phosphorus is 0.2-0.7g.
Preferably, the additive amount of hydrochloric acid solution is 4.6-10.5ml.
Preferably, the hydro-thermal reaction time 12-24h.
Preferably, during carbonization treatment, it is continually fed into the argon gas of 20ml/min.
Preferably, water and ethyl alcohol volume ratio are 1.5:1 in step (5).
The beneficial effects of the present invention are:
The present invention is fused together both functional element doping and mesoporous synthesis novelty, is realized synchronous preparation, is examined
Different phosphorus sources is examined, optimal with the effect of triphenyl phosphorus, triphenyl phosphorus is as important presoma, and the doping of only carbon does not mention
For phosphorus source, and the additive of mesoporous synthesis is served as, plays the role of reaming.Prepared material has uniform mesoporous knot
The advantages that structure, phosphorus doping effect is excellent, element good dispersion.
Detailed description of the invention
Fig. 1 is the images of transmissive electron microscope of phosphorus doping mesoporous carbon MC-TPP；
Fig. 2 is the small angle XRD diffraction patterns figure that triphenyl phosphorus makees the synthesising mesoporous carbon of additive；
Fig. 3 is the degree of graphitization diffraction patterns figure of meso-porous carbon material after phosphorus doping；
Fig. 4 is the N of sample2Absorption and pore size distribution result figure；
Fig. 5 is the Raman spectrogram of product phosphorus doping mesoporous carbon；
Fig. 6 is the C1s spectrogram of the XPS analysis of phosphorus doping mesoporous carbon MC-TPP；
Fig. 7 is the O1s spectrogram of the XPS analysis of phosphorus doping mesoporous carbon MC-TPP；
Fig. 8 is the P2p spectrogram of the XPS analysis of phosphorus doping mesoporous carbon MC-TPP；
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of preparation method of the meso-porous carbon material of phosphorus doping functionalization, comprises the following steps:
(1) 1.5g triblock copolymer is dissolved in 75ml distilled water first, 2g sucrose is added, dissolution is sufficiently stirred, then
0.7g triphenyl phosphorus and 15ml ethyl alcohol are added thereto, are stirred at room temperature uniformly, 6.9mL ethyl orthosilicate is then added, sufficiently stirs
Mix to obtain mixed liquor A；
(2) mixed liquor A is moved into single-necked flask, is stirred under 40 DEG C of water baths, with 0.5ml/min in whipping process
The hydrochloric acid solution of the 2mol/L of 4.6ml is added dropwise, is stirred overnight under the water bath, obtains mixed liquid B；
(3) mixed liquid B moving into autoclave, hydro-thermal reaction for 24 hours, after the reaction was completed, takes lower layer's product under the conditions of 373K,
It is dry under the conditions of 353K, obtain phosphorous composite precursor；
(4) by phosphorous composite precursor in high temperature Muffle furnace, carbonization treatment 2h under conditions of 574K, then by temperature
It is warming up to 1173K with the speed of 10K/min, keeps 3h；
Wherein, the argon gas of 20ml/min is continually fed into during carbonization treatment；
(5) under the conditions of 373K, the ethanol water containing sodium hydroxide for being 1.5:1 with volume ratio by step (4) products therefrom
Solution at reflux overnight removes silica, then continues the 12h that flows back with distilled water, finally with distilled water eccentric cleaning to solution
Aobvious neutrality, moves to vacuum oven drying, and sample is denoted as MC-TPP.
Embodiment 2:
A kind of preparation method of the meso-porous carbon material of phosphorus doping functionalization, comprises the following steps:
(1) 3g triblock copolymer is dissolved in 30ml distilled water first, 7.5g sucrose is added, dissolution is sufficiently stirred, then
0.2g triphenyl phosphorus and 30ml ethyl alcohol are added thereto, are stirred at room temperature uniformly, 3.4mL ethyl orthosilicate is then added, sufficiently stirs
Mix to obtain mixed liquor A；
(2) mixed liquor A is moved into single-necked flask, is stirred under 40 DEG C of water baths, with 0.5ml/min in whipping process
The hydrochloric acid solution of the 2mol/L of 10.5ml is added dropwise, is stirred overnight under the water bath, obtains mixed liquid B；
(3) mixed liquid B being moved into autoclave, hydro-thermal reaction 12h under the conditions of 373K takes lower layer's product after the reaction was completed,
It is dry under the conditions of 353K, obtain phosphorous composite precursor；
(4) by phosphorous composite precursor in high temperature Muffle furnace, carbonization treatment 2h under conditions of 574K, then by temperature
It is warming up to 1173K with the speed of 10K/min, keeps 3h；
Wherein, the argon gas of 20ml/min is continually fed into during carbonization treatment；
(5) under the conditions of 373K, the ethanol water containing sodium hydroxide for being 1.5:1 with volume ratio by step (4) products therefrom
Solution at reflux overnight removes silica, then continues the 12h that flows back with distilled water, finally with distilled water eccentric cleaning to solution
Aobvious neutrality, moves to vacuum oven drying, and sample is denoted as MC-TPP.
Embodiment 3:
A kind of preparation method of the meso-porous carbon material of phosphorus doping functionalization, comprises the following steps:
(1) 1.5g triblock copolymer is dissolved in 30ml distilled water first, 7.5g sucrose is added, dissolution is sufficiently stirred, so
It adds 0.7g triphenyl phosphorus and 15ml ethyl alcohol thereto afterwards, is stirred at room temperature uniformly, 3.4mL ethyl orthosilicate is then added, sufficiently
Stir to obtain mixed liquor A；
(2) mixed liquor A is moved into single-necked flask, is stirred under 40 DEG C of water baths, with 0.5ml/min in whipping process
The hydrochloric acid solution of the 2mol/L of 10.5ml is added dropwise, is stirred overnight under the water bath, obtains mixed liquid B；
(3) mixed liquid B moving into autoclave, hydro-thermal reaction for 24 hours, after the reaction was completed, takes lower layer's product under the conditions of 373K,
It is dry under the conditions of 353K, obtain phosphorous composite precursor；
(4) by phosphorous composite precursor in high temperature Muffle furnace, carbonization treatment 2h under conditions of 574K, then by temperature
It is warming up to 1173K with the speed of 10K/min, keeps 3h；
Wherein, the argon gas of 20ml/min is continually fed into during carbonization treatment；
(5) under the conditions of 373K, the ethanol water containing sodium hydroxide for being 1.5:1 with volume ratio by step (4) products therefrom
Solution at reflux overnight removes silica, then continues the 12h that flows back with distilled water, finally with distilled water eccentric cleaning to solution
Aobvious neutrality, moves to vacuum oven drying, and sample is denoted as MC-TPP.
Embodiment 4:
A kind of preparation method of the meso-porous carbon material of phosphorus doping functionalization, comprises the following steps:
(1) 3g triblock copolymer is dissolved in 75ml distilled water first, 2g sucrose is added, dissolution is sufficiently stirred, then to
0.2g triphenyl phosphorus and 30ml ethyl alcohol are wherein added, is stirred at room temperature uniformly, 6.9mL ethyl orthosilicate is then added, is sufficiently stirred
Obtain mixed liquor A；
(2) mixed liquor A is moved into single-necked flask, is stirred under 40 DEG C of water baths, with 0.5ml/min in whipping process
The hydrochloric acid solution of the 2mol/L of 4.6ml is added dropwise, is stirred overnight under the water bath, obtains mixed liquid B；
(3) mixed liquid B being moved into autoclave, hydro-thermal reaction 12h under the conditions of 373K takes lower layer's product after the reaction was completed,
It is dry under the conditions of 353K, obtain phosphorous composite precursor；
(4) by phosphorous composite precursor in high temperature Muffle furnace, carbonization treatment 2h under conditions of 574K, then by temperature
It is warming up to 1173K with the speed of 10K/min, keeps 3h；
Wherein, the argon gas of 20ml/min is continually fed into during carbonization treatment；
(5) under the conditions of 373K, the ethanol water containing sodium hydroxide for being 1.5:1 with volume ratio by step (4) products therefrom
Solution at reflux overnight removes silica, then continues the 12h that flows back with distilled water, finally with distilled water eccentric cleaning to solution
Aobvious neutrality, moves to vacuum oven drying, and sample is denoted as MC-TPP.
Embodiment 5:
A kind of preparation method of the meso-porous carbon material of phosphorus doping functionalization, comprises the following steps:
(1) 2g triblock copolymer is dissolved in 50ml distilled water first, 5g sucrose is added, dissolution is sufficiently stirred, then to
0.5g triphenyl phosphorus and 20ml ethyl alcohol are wherein added, is stirred at room temperature uniformly, 5mL ethyl orthosilicate is then added, is sufficiently stirred
Mixed liquor A；
(2) mixed liquor A is moved into single-necked flask, is stirred under 40 DEG C of water baths, with 0.5ml/min in whipping process
The hydrochloric acid solution of the 2mol/L of 5ml is added dropwise, is stirred overnight under the water bath, obtains mixed liquid B；
(3) mixed liquid B being moved into autoclave, hydro-thermal reaction 15h under the conditions of 373K takes lower layer's product after the reaction was completed,
It is dry under the conditions of 353K, obtain phosphorous composite precursor；
(4) by phosphorous composite precursor in high temperature Muffle furnace, carbonization treatment 2h under conditions of 574K, then by temperature
It is warming up to 1173K with the speed of 10K/min, keeps 3h；
Wherein, the argon gas of 20ml/min is continually fed into during carbonization treatment；
(5) under the conditions of 373K, the ethanol water containing sodium hydroxide for being 1.5:1 with volume ratio by step (4) products therefrom
Solution at reflux overnight removes silica, then continues the 12h that flows back with distilled water, finally with distilled water eccentric cleaning to solution
Aobvious neutrality, moves to vacuum oven drying, and sample is denoted as MC-TPP.
It is analyzed as follows with 1 gained sample MC-TPP of embodiment:
One, triphenyl phosphorus is the tem analysis of the synthesising mesoporous carbon material MC-TPP of phosphorus source
Such as Fig. 1, upper from figure as it can be seen that sample is mesoporous pattern, although pore structure is unordered, the size in hole is relatively uniform, mixes
The aperture about 7nm of mesoporous carbon after miscellaneous.Aperture is increased relative to the mesoporous material synthesized in the past, this is added with triphenyl phosphorus
Agent is related.Triphenyl phosphorus gets close to the hydrophobic part of surfactant as a kind of hydrophobic organic compound of low molecular weight, enters
The purpose of reaming is played in the hydrophobic side of micella.The sample structure that TEM figure is shown is similar to the vermicular texture of MSU-X.
Two, the small angle of phosphorus doping mesoporous carbon MC-TPP and Wide angle X-ray diffraction analysis
Fig. 2,3 are small angle XRD diffraction patterns that triphenyl phosphorus is the synthesising mesoporous carbon of additive.List is only observed from Fig. 2
One diffraction maximum, sample are the meso-hole structure of disordering.From the figure 3, it may be seen that nearby occur two diffraction maximums at 24 ° and 44 °, it is right respectively
Should be in the diffraction of (002) and (101) crystal face of graphite, meso-porous carbon material has certain degree of graphitization after illustrating phosphorus doping,
There is the crystallite of graphite to generate in its skeleton.
Three, the nitrogen adsorption analysis of phosphorus doping mesoporous carbon MC-TPP
Such as Fig. 4, it can be seen that Adsorption and desorption isotherms from the Adsorption and desorption isotherms in figure and belong to IV type adsorption isotherm,
The carbon sample of phosphorus doping synthesized by surface has typical meso-hole structure.The pore size distribution curve of adsorption isotherm is then intuitively given
The pore-size distribution situation of material intermediary hole out.From pore size distribution curve it is found that the pore-size distribution of material is relatively narrow, most Probable distrebution is straight
Diameter is 7.5nm, while there is also a large amount of micropores.
Four, the scanning electron microscope and Elemental redistribution of phosphorus doping mesoporous carbon MC-TPP
By carrying out electron scanning Electronic Speculum imaging analysis to synthetic sample, the sample of phosphorus doping be particle not of uniform size or
Person's agglomerate.The distribution diagram of element of phosphorus illustrates that phosphorus is not only successfully doped in mesoporous carbon, but also is distributed relatively uniform.Three kinds of elements
Content can be analyzed by X-ray energy spectrometer (XPS), and the content of three kinds of elements is respectively carbon 92.4at%, oxygen 7.2at%, phosphorus
0.4at%.
Five, the Raman spectrum analysis of phosphorus doping mesoporous carbon MC-TPP
There are two the characteristic peak of carbon, 1580cm for the Raman spectrum of general carbon material-1Locate (G mould) and 1350cm-1Locate (D mould).
It is the Raman spectrogram of product phosphorus doping mesoporous carbon such as Fig. 5, compared with the Raman map of pure graphite, doped samples
It is all significantly broadened at the peak of G and D band, illustrate to contain more amorphous carbon in sample.
Six, the XPS analysis of phosphorus doping mesoporous carbon MC-TPP
Such as Fig. 6-8, x-ray photoelectron spectroscopy test is carried out to phosphorus doping mesoporous carbon sample, wherein phosphorus, oxygen, carbon
The combination energy and element of C1s, P2p and O1s belong to list 1:
Table 1
The peak C1s in Fig. 6, the peak of C1s is asymmetric peak shape, shows to contain complexity in carbon surface in 284.7eV when not being fitted
Carbon species, this is because the surface layer in mesoporous carbon has caused by oxygen-containing functional group.By Gauss curve fitting, C1s spectrogram can be divided
At three peaks, it is located at 284.6eV, 285.3eV, 288.9eV, the halfwidth at each peak after fitting is respectively 0.9eV,
2.2eV, 6.3eV.Other than main peak 284.6eV belongs to graphite linings carbon, other two acromions are respectively belonging to hydroxyl or ether
In C-O, carbonyl (C=O).Phosphorus compound can not be determined from the combination of C1s, this is because the electron binding energy class of C-O-P
Be similar to the combination energy of alcohol or ether functional group, and the C1s of the phosphonate containing C-P key or compound combine can just between
Between graphitic carbon and the electron binding energy of oxygen-containing carbon.
Momentum profiles Fig. 8 of P2p is as it can be seen that the peak 2p of phosphorus is very weak from phosphorus doping mesoporous carbon sample, and signal-to-noise ratio is low, with phosphorus
Content is lower in relation to (content of phosphorus is 0.67%).Peak is located at 132.8eV, and peak shape is wider, by being fitted to peak, peak center
Positioned at 133eV.Oxide-phosphorus pentoxide base peak electron binding energy peak (136.0eV) relative to phosphorus is toward low energy direction
Mobile, this illustrates that the chemical environment of the phosphorus in synthetic sample is different from the chemical state of phosphorus species in phosphorus pentoxide substance.Consider
It is triphenyl phosphorus to phosphorus presoma, phosphorus exists in the form of C-P, and carbon phosphorus participates in carbon graphite process, phosphorus part in subsequent roasting
Doping enters in the network structure of carbon, and there are also part keys combined with oxygen.
Different phosphate sources comparison
Select the mixture of triphenyl phosphorus and inorganic phos phoric acid and the two suitable proportion for the forerunner of preparation doping phosphorus
Body, comparison optimization.Wherein, structure of the pattern of synthesized mesoporous carbon using triphenyl phosphorus as phosphorus source is optimal, and is with phosphoric acid
Source is difficult to be doped into carbon material, and triphenyl phosphorus relatively easily realizes doping of the phosphorus in carbon.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (6)
1. a kind of preparation method of the meso-porous carbon material of phosphorus doping functionalization, which is characterized in that comprise the following steps:
(1) 1.5-3g triblock copolymer is dissolved in 30-75ml distilled water first, 2-7.5g sucrose is added, dissolution is sufficiently stirred,
Then appropriate triphenyl phosphorus and 15-30ml ethyl alcohol are added thereto, are stirred at room temperature uniformly, the positive silicic acid of 3.4-6.9mL is then added
Mixed liquor A is sufficiently stirred to obtain in ethyl ester；
(2) mixed liquor A is moved into single-necked flask, stirs under 40 DEG C of water baths, is added dropwise in whipping process with 0.5ml/min
The hydrochloric acid solution of a certain amount of 2mol/L is stirred overnight under the water bath, obtains mixed liquid B；
(3) mixed liquid B is moved into autoclave, hydro-thermal reaction certain time takes lower layer to produce after the reaction was completed under the conditions of 373K
Object, it is dry under the conditions of 353K, obtain phosphorous composite precursor；
(4) by phosphorous composite precursor in high temperature Muffle furnace, carbonization treatment 2h under conditions of 574K, then by temperature with
The speed of 10K/min is warming up to 1173K, keeps 3h；
(5) under the conditions of 373K, step (4) products therefrom is refluxed overnight with the ethanol water containing sodium hydroxide, removal two
Then silica continues the 12h that flows back with distilled water, finally move to vacuum drying to the aobvious neutrality of solution with distilled water eccentric cleaning
Case is dry, and sample is denoted as MC-TPP.
2. the preparation method of the meso-porous carbon material of phosphorus doping functionalization according to claim 1, which is characterized in that triphenyl
The additive amount of phosphorus is 0.2-0.7g.
3. the preparation method of the meso-porous carbon material of phosphorus doping functionalization according to claim 1, which is characterized in that hydrochloric acid is molten
The additive amount of liquid is 4.6-10.5ml.
4. the preparation method of the meso-porous carbon material of phosphorus doping functionalization according to claim 1, which is characterized in that hydro-thermal is anti-
It is 12-24h between seasonable.
5. the preparation method of the meso-porous carbon material of phosphorus doping functionalization according to claim 1, which is characterized in that at carbonization
During reason, it is continually fed into the argon gas of 20ml/min.
6. the preparation method of the meso-porous carbon material of phosphorus doping functionalization according to claim 1, which is characterized in that the step
Suddenly water and ethyl alcohol volume ratio are 1.5:1 in (5).
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| CN109970040A (en) * | 2019-05-08 | 2019-07-05 | 贵州大学 | A method of mesoporous carbon is prepared by carbon nitrogen source double-driving force of chitosan |
| CN111744513A (en) * | 2020-07-07 | 2020-10-09 | 上海大学 | Phosphorus doped carbon-based catalyst and application thereof |
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