CN109876841A - A kind of method of 2- amino terephthalic acid (TPA) and amine compounds combined polymerization preparation graphite phase carbon nitride visible light catalyst - Google Patents
A kind of method of 2- amino terephthalic acid (TPA) and amine compounds combined polymerization preparation graphite phase carbon nitride visible light catalyst Download PDFInfo
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- CN109876841A CN109876841A CN201910058788.4A CN201910058788A CN109876841A CN 109876841 A CN109876841 A CN 109876841A CN 201910058788 A CN201910058788 A CN 201910058788A CN 109876841 A CN109876841 A CN 109876841A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A kind of method of 2- amino terephthalic acid (TPA) and amine compounds combined polymerization preparation graphite phase carbon nitride visible light catalyst, after mixing by amine compounds and 2- amino terephthalic acid (TPA), obtain mixed-powder, then mixed-powder is calcined at 520-600 DEG C, obtains graphite phase carbon nitride visible light catalyst.Preparation method involved by the present invention is simple, and gained novel graphite phase carbon nitride has the better visible light catalytic H2-producing capacity of more original carbonitride.
Description
Technical field
The present invention relates to a kind of 2- amino terephthalic acid (TPA)s and amine compounds combined polymerization to prepare graphite phase carbon nitride visible light
The method of catalyst belongs to energy and material preparation and photocatalysis field.
Background technique
Mankind nowadays society faces the shortage of the energy and the environment two large problems energy and the seriously polluted of environment restricts people
The development of class society.On the one hand, social high speed development makes the mankind increasing for the demand of the energy, and our current institutes
The energy still based on traditional fossil fuel, but because fossil fuel it is non-renewable so that it must have exhaustion
One day.On the other hand, the burning of fossil fuel causes serious environmental pollution and the harm to environment, such as greenhouse effects, acid
Rain, photochemical fog etc. produce serious threat to the existence of the mankind.Therefore, a kind of sustainable substitution of cleaning is found
The energy becomes more urgent.And China has a vast territory, possesses solar energy resources extremely abundant, potentiality to be exploited is huge, from long-range
It can satisfy the demand of national sustainable development from the point of view of development completely.But solar energy density is low, it is dispersed it is strong, unstable,
Discontinuous disadvantage makes us still lack the effective means utilized on a large scale to its high efficiency, low cost so far.Early in 1972,
Japanese scholars Fujishima and Honda is to illumination TiO2Electrode leads to the discovery of water decomposition generation hydrogen, so that solar energy converts
Become reality for Hydrogen Energy, also to provide an ideal approach using the solution of all difficulties during solar energy.And it is sharp
A kind of Solar use mode of great potential is considered to be with solar energy photocatalytic hydrogen production by water decomposition, the hydrogen produced is again
A kind of tasteless nontoxic clean fuel of no color or smell, have energy storage density it is high, it is pollution-free, be easy to mutually convert with electric energy etc. it is excellent
Point is considered as a kind of ideal alternative energy source.
Ideal graphite phase carbon nitride (g-C3N4) it is a kind of N-shaped organic polymer semiconductor, there is triazine ring structure, C is former
Son and N atomic ordered are staggered.Since the material preparation method is convenient, low in cost, chemical stability is good, and have
Suitable forbidden bandwidth (2.7eV) and bandedge placement meet the needs that visible light catalytic decomposes water reaction, therefore more next in recent years
More by the favor of educational circles.2008, Wang etc. reported g-C for the first time3N4Visible light catalytic hydrogen production potential, result of study table
It is bright, g-C3N4Can be artificial synthesized using the method realization of high-temperature polycondensation between 400 DEG C and 600 DEG C, and pass through band structure
It calculates and analytical proof g-C3N4Visible light catalytic ability, this is absorbed for it visible light and restores H+ to generate H2It provides
It ensures, becomes the research hotspot for producing hydrogen photochemical catalyst.But g-C3N4Internal synusia is not necessarily to ideal graphite-phase and carries out
Arrangement, but synusia occurs and stacks, therefore practical specific surface area is often lower, and light excites generated electron hole pair multiple
It closes too fast, cannot effectively restore hydrogen ion.The above reason leads to g-C3N4Photocatalytic activity it is lower, there is an urgent need to find row
Effective method of modifying further increases Photocatalyzed Hydrogen Production ability.
Summary of the invention
The object of the present invention is to provide a kind of 2- amino terephthalic acid (TPA)s and amine compounds combined polymerization to prepare graphite-phase
The visible light catalytic performance of the method for carbonitride visible light catalyst, the combined polymerization graphite phase carbon nitride of this method preparation obviously mentions
Height is about 3.2 times of original graphite phase carbon nitride, and preparation method is simple.
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of side of 2- amino terephthalic acid (TPA) and amine compounds combined polymerization preparation graphite phase carbon nitride visible light catalyst
Method after mixing by amine compounds and 2- amino terephthalic acid (TPA) obtains mixed-powder, then by mixed-powder in 520-
It is calcined at 600 DEG C, obtains graphite phase carbon nitride visible light catalyst.
A further improvement of the present invention lies in that amine compounds are at least one of urea, melamine, dicyandiamide.
A further improvement of the present invention lies in that the mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is (0.1-1):
1000。
A further improvement of the present invention lies in that the mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is (0.1-0.5):
1000。
A further improvement of the present invention lies in that the mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is 0.3:1000.
A further improvement of the present invention lies in that calcining is carried out in ash content furnace.
A further improvement of the present invention lies in that calcining is carried out under air atmosphere.
A further improvement of the present invention lies in that the time of calcining is 2-5 hours.
A further improvement of the present invention lies in that with 3-5 DEG C/min of heating rate from room temperature to 520-600 DEG C.
A further improvement of the present invention lies in that the detailed process of amine compounds and the mixing of 2- amino terephthalic acid (TPA) are as follows: will
Amine compounds are add to deionized water with 2- amino terephthalic acid (TPA), and after dissolution forms clear solution, stirring is steamed under heating
Dry, gained powder is uniform with mortar grinder again, obtains mixed-powder.
Compared with prior art, the invention has the benefit that
The present invention provides a kind of novel graphite phase carbon nitride visible light catalysts of combined polymerization preparation, pass through amine compounds
It, can synthesizing new g-C on a molecular scale with the combined polymerization of 2- amino terephthalic acid (TPA)3N4Photochemical catalyst.It is anti-by combined polymerization
It answers, chemical composition, the regulation semiconductor energy band structure of catalyst can be optimized, improve absorbing properties and improve photo-generated carrier point
From efficiency, the activity of photocatalysis Decomposition aquatic products hydrogen is substantially increased.Specifically have the advantage that
1) synthesis process is simple, and not generation environment contaminating by-products；
2) using amine compounds and minute quantity 2- amino to benzene dibenzoic acid as presoma, it is low in cost；
3) gained sample significantly improves visible light catalytic and decomposes aquatic products hydrogen activity, is the pact of original graphite phase carbon nitride
3.2 again.
Detailed description of the invention
Fig. 1 is the molecular structural formula of 2- amino terephthalic acid (TPA) used in the present invention.
The copolymerization for the different proportion 2- amino terephthalic acid (TPA) that Fig. 2 is comparative example 1 of the present invention, embodiment 1-5 is prepared
Close the X-ray diffractogram of the novel graphite phase carbon nitride of preparation.
The copolymerization for the different proportion 2- amino terephthalic acid (TPA) that Fig. 3 is comparative example 1 of the present invention, embodiment 1-5 is prepared
Close the UV-vis absorption spectrum figure of the novel graphite phase carbon nitride of preparation.
Fig. 4 is the transmission electron microscope image for the CN-3.0 that the embodiment of the present invention 1 is prepared
The copolymerization for the different proportion 2- amino terephthalic acid (TPA) that Fig. 5 is comparative example 1 of the present invention, embodiment 1-5 is prepared
Close the visible light H2-producing capacity figure of the novel graphite phase carbon nitride of preparation.
Specific embodiment
The present invention is further illustrated below in conjunction with attached drawing and embodiment, it should be appreciated that following drawings and the embodiments are only
For illustrating the present invention, it is not intended to limit the present invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
2- amino terephthalic acid (TPA) (referring to Fig. 1) of the invention and amine compounds combined polymerization preparation graphite phase carbon nitride are visible
The method of photochemical catalyst are as follows: after mixing by amine compounds and 2- amino terephthalic acid (TPA), obtain mixed-powder, then will mix
It closes powder to be put into crucible, capping is calcined in ash content furnace with air atmosphere, with 3-5 DEG C/min of heating rate from room temperature
It is calcined 2-5 hours to 520-600 DEG C and at 520-600 DEG C, obtains graphite phase carbon nitride visible light catalyst.
Wherein, amine compounds are one or more of urea, melamine, dicyandiamide.
The mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is (0.1-1): 1000.
Preferably, the mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is (0.1-0.5): 1000.
It is furthermore preferred that the mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is 0.3:1000.
The detailed process of amine compounds and the mixing of 2- amino terephthalic acid (TPA) are as follows: by amine compounds and 2- amino terephthaldehyde
Acid is add to deionized water, and after dissolution forms clear solution, stirring is evaporated under heating, and gained powder is equal with mortar grinder again
It is even, obtain mixed-powder.Amine compounds and 2- amino terephthalic acid (TPA) can also be mixed directly, obtain mixed-powder.
Comparative example 1
10g urea is dissolved in the deionized water of 20mL, transparent mixed solution is formed, is stirred in 70 DEG C of water-bath
It is evaporated.Gained compounding substances are ground uniformly in mortar, are added in 50mL crucible with cover, crucible is then placed in ash content
Furnace is kept for 4 hours, cooled to room temperature with 5 DEG C/min of heating rate from room temperature to 550 DEG C.It is copolymerized
Close novel graphite phase carbon nitride, pending performance test.
Embodiment 1
The 2- amino terephthalic acid (TPA) of 10g urea and 0.5mg are dissolved in the deionized water of 20mL, transparent mixing is formed
Solution is stirred in 70 DEG C of water-bath and is evaporated.Gained compounding substances are ground uniformly in mortar, are added to 50mL earthenware with cover
In crucible, crucible is then placed in ash content furnace, with 5 DEG C/min of heating rate from room temperature to 550 DEG C, is kept for 4 hours, from
So it is cooled to room temperature.Obtain combined polymerization novel graphite phase carbon nitride, pending performance test.
Embodiment 2
The 2- amino terephthalic acid (TPA) of 10g urea and 1mg are dissolved in the deionized water of 20mL, it is molten to form transparent mixing
Liquid is stirred in 70 DEG C of water-bath and is evaporated.Gained compounding substances are ground uniformly in mortar, are added to 50mL crucible with cover
In, crucible is then placed in ash content furnace, with 5 DEG C/min of heating rate from room temperature to 550 DEG C, is kept for 4 hours, it is natural
It is cooled to room temperature.Obtain combined polymerization novel graphite phase carbon nitride, pending performance test.
Embodiment 3
The 2- amino terephthalic acid (TPA) of 10g urea and 3mg are dissolved in the deionized water of 20mL, it is molten to form transparent mixing
Liquid is stirred in 70 DEG C of water-bath and is evaporated.Gained compounding substances are ground uniformly in mortar, are added to 50mL crucible with cover
In, crucible is then placed in ash content furnace, with 5 DEG C/min of heating rate from room temperature to 550 DEG C, is kept for 4 hours, it is natural
It is cooled to room temperature.Obtain combined polymerization novel graphite phase carbon nitride, pending performance test.
Embodiment 4
The 2- amino terephthalic acid (TPA) of 10g urea and 5mg are dissolved in the deionized water of 20mL, it is molten to form transparent mixing
Liquid is stirred in 70 DEG C of water-bath and is evaporated.Gained compounding substances are ground uniformly in mortar, are added to 50mL crucible with cover
In, crucible is then placed in ash content furnace, with 5 DEG C/min of heating rate from room temperature to 550 DEG C, is kept for 4 hours, it is natural
It is cooled to room temperature.Obtain combined polymerization novel graphite phase carbon nitride, pending performance test.
Embodiment 5
The 2- amino terephthalic acid (TPA) of 10g urea and 7mg are dissolved in the deionized water of 20mL, it is molten to form transparent mixing
Liquid is stirred in 70 DEG C of water-bath and is evaporated.Gained compounding substances are ground uniformly in mortar, are added to 50mL crucible with cover
In, crucible is then placed in ash content furnace, with 5 DEG C/min of heating rate from room temperature to 550 DEG C, is kept for 4 hours, it is natural
It is cooled to room temperature.Obtain combined polymerization novel graphite phase carbon nitride, pending performance test.
Embodiment 6
After mixing by amine compounds and 2- amino terephthalic acid (TPA), mixed-powder is obtained, then puts mixed-powder
Enter in crucible, capping is calcined in ash content furnace with air atmosphere, to 600 DEG C and is forged with 3 DEG C/min of heating rates from room temperature
It burns 2 hours, obtains graphite phase carbon nitride visible light catalyst.
Wherein, amine compounds are melamine.
The mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is 0.2:1000.
Embodiment 7
After mixing by amine compounds and 2- amino terephthalic acid (TPA), mixed-powder is obtained, then puts mixed-powder
Enter in crucible, capping is calcined in ash content furnace with air atmosphere, to 570 DEG C and is forged with 4 DEG C/min of heating rates from room temperature
It burns 3 hours, obtains graphite phase carbon nitride visible light catalyst.
Wherein, amine compounds are the mixture of melamine and dicyandiamide.
The mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is 0.6:1000.
Embodiment 8
After mixing by amine compounds and 2- amino terephthalic acid (TPA), mixed-powder is obtained, then puts mixed-powder
Enter in crucible, capping is calcined in ash content furnace with air atmosphere, to 570 DEG C and is forged with 4 DEG C/min of heating rates from room temperature
It burns 3 hours, obtains graphite phase carbon nitride visible light catalyst.
Wherein, amine compounds are the mixture of urea, melamine and dicyandiamide.
The mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is 0.3:1000.
Referring to fig. 2, figure it is seen that corresponding to g-C with 2 θ=27.4 °3N4(002) crystal face, belong to pi-conjugated flat
The class graphite laminate in face is accumulated, the corresponding g-C in 2 θ=13.0 °3N4(100) crystal face, belong to the repetition primitive of seven piperazine rings.And it is total to
Polymerization reaction destroys g-C there is no obvious3N4Packed structures and connection type.
Referring to Fig. 3, from figure 3, it can be seen that combined polymerization is prepared new with the increase of 2- amino terephthalic acid (TPA) additive amount
Type g-C3N4Absorbing properties be obviously improved.
Referring to fig. 4, from fig. 4, it can be seen that there are apparent hole, more original carbonitride lamella in the surface of CN-3.0 sample
Obvious thinning, this facilitates the separation of carrier.
Comparative example 1, implementation 1-5 the combined polymerization novel graphite phase carbon nitride being prepared are carried out in accordance with the following steps visible
Photocatalyzed Hydrogen Production performance test:
The novel graphite phase carbon nitride visible light catalytic of 10mg combined polymerization preparation is added in the reactor that volume is 110mL
Agent adds the deionized water of 72mL, 8mL triethanolamine is added as sacrifice agent, 500 μ L mass concentrations containing Pt, which are added, is
The H of 0.5978mg/mL2PtCl6Solution carries out light deposition co-catalyst Pt.It is passed through nitrogen in illumination forward reaction device and purges 15 points
Clock, to remove the oxygen in solution.300W xenon lamp is opened, 420nm edge filter is added, opens magnetic stirrer reactor
In solution, the H of generation2It is detected using gas-chromatography.As shown in figure 5, for different proportion 2- amino terephthalic acid (TPA)
The visible light H2-producing capacity figure of the novel graphite phase carbon nitride of combined polymerization preparation.Abscissa indicates that 2- amino is to benzene two in presoma
The content of formic acid, respectively 0mg, 0.5mg, 1mg, 3mg, 5mg, 7mg, ordinate are generation rate (μm olh of hydrogen-1·
gcat -1).As can be seen that the novel graphite phase carbon nitride that the combined polymerization preparation of the 2- amino terephthalic acid (TPA) of 3mg is added produces hydrogen and lives
Property highest, reaches 10600 μm of olh-1·gcat -1, and the production hydrogen activity of original carbon nitride material is 3323 μm of olh-1·
gcat -1.It can be seen that the more original carbonitride of novel graphite phase carbon nitride catalytic activity of gained combined polymerization preparation has obviously
Raising, hydrogen-producing speed is about 3.2 times of original carbonitride.
Method and core technology of the invention that the above embodiments are only used to help understand, is not to the application
Scope limitation.For those skilled in the art, all any modifications within the application principle, replacement, improve etc.,
Within the scope of protection of this application.
Claims (10)
1. a kind of method of 2- amino terephthalic acid (TPA) and amine compounds combined polymerization preparation graphite phase carbon nitride visible light catalyst,
It is characterized in that, after mixing by amine compounds and 2- amino terephthalic acid (TPA), mixed-powder is obtained, then by mixed-powder
It is calcined at 520-600 DEG C, obtains graphite phase carbon nitride visible light catalyst.
2. a kind of 2- amino terephthalic acid (TPA) according to claim 1 and amine compounds combined polymerization prepare graphite phase carbon nitride
The method of visible light catalyst, which is characterized in that amine compounds are at least one of urea, melamine, dicyandiamide.
3. a kind of 2- amino terephthalic acid (TPA) according to claim 1 and amine compounds combined polymerization prepare graphite phase carbon nitride
The method of visible light catalyst, which is characterized in that the mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is (0.1-1):
1000。
4. a kind of 2- amino terephthalic acid (TPA) according to claim 1 or 3 and amine compounds combined polymerization prepare graphite-phase nitrogen
Change the method for carbon visible light catalyst, which is characterized in that the mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is (0.1-
0.5):1000。
5. a kind of 2- amino terephthalic acid (TPA) according to claim 4 and amine compounds combined polymerization prepare graphite phase carbon nitride
The method of visible light catalyst, which is characterized in that the mass ratio of 2- amino terephthalic acid (TPA) and amine compounds is 0.3:1000.
6. a kind of 2- amino terephthalic acid (TPA) according to claim 1 and amine compounds combined polymerization prepare graphite phase carbon nitride
The method of visible light catalyst, which is characterized in that calcining is carried out in ash content furnace.
7. a kind of 2- amino terephthalic acid (TPA) according to claim 1 and amine compounds combined polymerization prepare graphite phase carbon nitride
The method of visible light catalyst, which is characterized in that calcining is carried out under air atmosphere.
8. a kind of 2- amino terephthalic acid (TPA) according to claim 1 and amine compounds combined polymerization prepare graphite phase carbon nitride
The method of visible light catalyst, which is characterized in that the time of calcining is 2-5 hours.
9. a kind of 2- amino terephthalic acid (TPA) according to claim 1 and amine compounds combined polymerization prepare graphite phase carbon nitride
The method of visible light catalyst, which is characterized in that with 3-5 DEG C/min of heating rate from room temperature to 520-600 DEG C.
10. a kind of 2- amino terephthalic acid (TPA) according to claim 1 and amine compounds combined polymerization prepare graphite-phase nitridation
The method of carbon visible light catalyst, which is characterized in that the detailed process of amine compounds and the mixing of 2- amino terephthalic acid (TPA) are as follows: will
Amine compounds are add to deionized water with 2- amino terephthalic acid (TPA), and after dissolution forms clear solution, stirring is steamed under heating
Dry, gained powder is uniform with mortar grinder again, obtains mixed-powder.
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| CN110639585A (en) * | 2019-09-19 | 2020-01-03 | 浙江大学 | Copolymerization modified layered graphite phase carbon nitride photocatalyst and preparation method and application thereof |
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| CN110639585A (en) * | 2019-09-19 | 2020-01-03 | 浙江大学 | Copolymerization modified layered graphite phase carbon nitride photocatalyst and preparation method and application thereof |
| CN110813347A (en) * | 2019-10-14 | 2020-02-21 | 西安交通大学 | Molecular doping modified graphite phase carbon nitride photocatalyst with three-dimensional loose structure and preparation method and application thereof |
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| CN113600239A (en) * | 2021-08-09 | 2021-11-05 | 华侨大学 | Triptycene modified graphite-phase carbon nitride and preparation method and application thereof |
| CN113600239B (en) * | 2021-08-09 | 2023-04-11 | 华侨大学 | Triptycene modified graphite-phase carbon nitride and preparation method and application thereof |
| CN113813979A (en) * | 2021-09-22 | 2021-12-21 | 吉林医药学院 | Method for improving graphite-phase carbon nitride photocatalytic performance by molecular doping means |
| CN113942983A (en) * | 2021-10-19 | 2022-01-18 | 陕西科技大学 | Preparation method of novel carbon nitride-based material combining copolymerization and thermal induction |
| CN116656369A (en) * | 2023-07-14 | 2023-08-29 | 广州绿固环保科技有限公司 | Severely contaminated soil restoration agent and preparation method and restoration method thereof |
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