CN107008482A - A kind of photochemical catalyst without metallic element that can be used under no light condition and preparation method thereof - Google Patents
A kind of photochemical catalyst without metallic element that can be used under no light condition and preparation method thereof Download PDFInfo
- Publication number
- CN107008482A CN107008482A CN201710229252.5A CN201710229252A CN107008482A CN 107008482 A CN107008482 A CN 107008482A CN 201710229252 A CN201710229252 A CN 201710229252A CN 107008482 A CN107008482 A CN 107008482A
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- photochemical catalyst
- dispersion liquid
- graphene
- cnt
- metallic element
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- 239000003054 catalyst Substances 0.000 title claims abstract description 48
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 27
- 230000001699 photocatalysis Effects 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000007306 functionalization reaction Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000006185 dispersion Substances 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 25
- 239000002041 carbon nanotube Substances 0.000 claims description 17
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 17
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 238000007146 photocatalysis Methods 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 239000002159 nanocrystal Substances 0.000 claims description 5
- 239000002356 single layer Substances 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000005286 illumination Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 102100021470 Solute carrier family 28 member 3 Human genes 0.000 abstract 1
- 101710186856 Solute carrier family 28 member 3 Proteins 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
Abstract
The present invention discloses a kind of photochemical catalyst without metallic element that can be used under no light condition, it is characterised in that：Described photochemical catalyst is made up of the raw material of following mass fraction：The CNT 3 15 of functionalization, graphene 15, carbonitride 20 60.It also still keeps photocatalytic activity compared with traditional photochemical catalyst even if without illumination.While the method disclosed by the invention for preparing this kind of photochemical catalyst, technique simple possible, and without expensive equipment, it is convenient, flexible, beneficial to operation and popularization, it can be said that the photochemical catalyst without metallic element that this kind can be used under no light condition possesses a variety of advantages, it is particularly suitable for popularization and application in the art, its market prospects is very wide.
Description
Technical field
The present invention relates to photocatalysis technology field, particularly it is a kind of can be used under no light condition without metallic element
Photochemical catalyst, and this kind of photochemical catalyst preparation method.
Background technology
Energy crisis and environmental pollution are two the main themes of global concern, and photocatalytic process can convert solar energy
For chemical energy and environmental contaminants are removed, therefore the development of photochemical catalyst is focus of concern.However, traditional photocatalysis
Agent must can just work under conditions of illumination, and this causes photocatalysis technology to be restricted in many practical applications.If
Can prepare it is a kind of the photochemical catalyst of photocatalytic activity can be kept in the case where having light and no light condition, will be enlarged by it is light-catalysed should
With category, the development of photochemical catalyst and photocatalysis field is more beneficial for.
The content of the invention
The present invention is in order to solve the above-mentioned deficiency present in prior art, to propose that one kind still can be with no light condition
Use, and the photochemical catalyst without metallic element, while also disclosing the preparation method of this kind of photochemical catalyst.
The present invention technical solution be：A kind of photocatalysis without metallic element that can be used under no light condition
Agent, it is characterised in that：Described photochemical catalyst is made up of the raw material of following mass fraction：
The CNT 3-15 of functionalization
Graphene 1-5
Carbonitride 20-60.
A kind of method for preparing the photochemical catalyst without metallic element that can be used as described above under no light condition, its
It is characterised by：Described method is followed the steps below：
CNT is put into the mixed liquor of 14.5mol/L concentrated nitric acid and the 18.4mol/L concentrated sulfuric acid first, and dense nitre
The volume ratio of acid and the concentrated sulfuric acid is 1:3, and mixed liquor is heated to 60-80 DEG C, and be incubated 2-6h, mixed liquor is carried out suction filtration or
Person's centrifugal treating, is washed out, up to neutral, obtaining the CNT of functionalization,
Then it is 3 the CNT of functionalization to be put into volume ratio:In 2 water and the mixed liquor of isopropanol, 2- is persistently stirred
6h, obtains carbon nano tube dispersion liquid, and ensures in carbon nano tube dispersion liquid, and the concentration of CNT is 9-18mg/mL, then
Graphene is added into carbon nano tube dispersion liquid, and 3-5h is persistently stirred on magnetic stirring apparatus, ultrasonically treated 2-4h, is obtained afterwards
Carbon nano tube/graphene dispersion liquid is obtained, carbonitride is put into carbon nano tube/graphene dispersion liquid, ultrasonically treated 1-5h is obtained
Whole dispersion liquid, by whole dispersion liquid under conditions of 140-180 DEG C hydro-thermal reaction 10-24h, then naturally cool to room temperature ,-
2-12h is freeze-dried under conditions of 50 to -20 DEG C, that is, obtains photochemical catalyst.
Described graphene is graphene oxide or redox graphene.
Described carbonitride is the carbonitride of nanocrystal monolayer or the carbonitride of nanometer multilayer.
The present invention compared with the existing technology, has the following advantages that：
The photochemical catalyst without metallic element disclosed in this invention that can be used under no light condition, with traditional photochemical catalyst
Compare, the illumination of incident light stops in photocatalytic process, and this kind of photochemical catalyst is maintained to photocatalytic activity.This
The disclosed photochemical catalyst of invention both can also be used as incident light by the use of ultraviolet light as incident light by the use of visible ray.It
Using CNT and graphene as photochemical catalyst composition material, it is possible to achieve the storage of light induced electron, under illumination condition,
Light induced electron can be stored in catalyst by photochemical catalyst；And when unglazed irradiation, the light induced electron of storage is discharged again
Come, reality is carried out now with the purpose of photocatalytic activity can be kept under light and no light condition using this principle.Simultaneously as metal
The scarcity of element, causes the price containing metallic element material of a relatively high.And the nonmetallic member including carbon, nitrogen, oxygen
Element rich reserves on earth, therefore the holistic cost of this kind of photochemical catalyst can also be controlled in a relatively low scope.Together
When, the method disclosed in this invention for preparing this photochemical catalyst, its technique simple possible, without any expensive equipment, and
Beneficial to operation and popularization, it can be said that this photochemical catalyst and preparation method thereof possesses a variety of advantages, its market prospects ten
Divide wide.
Brief description of the drawings
Fig. 1 is the scanning electron microscopic picture of photochemical catalyst of the present invention.
Fig. 2 is the transmission electron microscope picture of photochemical catalyst of the present invention.
Embodiment
Below in conjunction with the embodiment of the brief description of the drawings present invention.As shown in Figure 1 and Figure 2：One kind can be in no light condition
The lower photochemical catalyst without metallic element used, is made up of the raw material of following mass fraction：The CNT 3-15 of functionalization
Part, 1-5 parts of graphene, 20-60 parts of carbonitride, graphene here can be graphene oxide or redox graphene；This
In carbonitride can be nano level individual layer carbonitride, or the carbonitride of nano level multilayer；
A kind of method for preparing the photochemical catalyst without metallic element that can be used as described above under no light condition, according to
Lower step is carried out：
CNT is put into concentrated nitric acid first（14.5 mol/L）And the concentrated sulfuric acid（18.4 mol/L）Mixed liquor in, it is above-mentioned
Concentrated nitric acid and the concentrated sulfuric acid volume ratio be 1:3, and mixed liquor is heated to 80 DEG C, and 2-6h is incubated, mixed liquor is taken out
Filter or centrifugal treating, are washed out, up to neutral, obtaining the CNT of functionalization,
Then it is 3 the CNT of functionalization to be put into volume ratio:In 2 water and the mixed liquor of isopropanol, 2- is persistently stirred
6h, obtains carbon nano tube dispersion liquid, it is necessary to ensure in carbon nano tube dispersion liquid, and the concentration of CNT is 9-18mg/mL, so
Graphene is added in backward carbon nano tube dispersion liquid, and persistently stirs on magnetic stirring apparatus 3-5h, afterwards ultrasonically treated 2-4h,
Carbon nano tube/graphene dispersion liquid is obtained, carbonitride is put into carbon nano tube/graphene dispersion liquid, ultrasonically treated 1-5h,
Obtain whole dispersion liquid, by whole dispersion liquid under conditions of 140-180 DEG C hydro-thermal reaction 10-24h, then naturally cool to room temperature,
And 2-12h is freeze-dried under conditions of -50 to -20 DEG C, that is, obtain photochemical catalyst.
Embodiment：
Take the raw material of following mass fraction：CNT 0.9g, graphene oxide 0.3g, nanocrystal monolayer carbonitride 3.6g,
Using water and isopropanol mixture as dispersant, by CNT, graphene oxide, the mixing of nanocrystal monolayer carbonitride is equal
It is even, the photochemical catalyst without metallic element that can be used under no light condition is prepared by hydro-thermal reaction, specific method is as follows：
CNT is added to the mixed liquor of concentrated nitric acid and the concentrated sulfuric acid first（Wherein the volume ratio of concentrated nitric acid and the concentrated sulfuric acid is 1:3）
In, and it is heated to 80 DEG C, 4 hours are incubated, is washed after vacuum filtration, obtains the CNT of functionalization；
The CNT of 0.9g functionalization is put into cumulative volume in 60mL water and the mixture of isopropanol（Its reclaimed water and
The volume ratio of isopropanol is 3:2）, 3h is persistently stirred, the CNT of standby function disperses in the mixture of water and isopropanol
After uniform, that is, carbon nano tube dispersion liquid is obtained, then 0.3g graphene oxide is put into carbon nano tube dispersion liquid, and
3h is persistently stirred, afterwards ultrasonically treated 4h, after being uniformly dispersed, 3.6g nanocrystal monolayer carbonitride is added thereto, is stirred in magnetic force
Mix and 3h is persistently stirred on device, ultrasonically treated 5h, until forming finely dispersed whole dispersion liquid；
Above-mentioned whole dispersion liquid is put into pyroreaction kettle, the hydro-thermal reaction 24h under conditions of 150 DEG C, then natural cooling
To room temperature, 10h is freeze-dried under conditions of -45 DEG C, that is, obtains the light without metallic element that can be used under no light condition
Catalyst.
Analysis on Mechanism to photocatalytic process understands that light induced electron is the key for starting light-catalyzed reaction.If preparing one
Catalyst is planted, under illumination condition, light induced electron can be stored in catalyst by photochemical catalyst；When unglazed irradiation, storage
Light induced electron discharge again, it is possible to it is real now with photocatalytic activity can be kept under light and no light condition.The present invention
Described photochemical catalyst is namely based on above-mentioned idea, using capacitance material as a part for photochemical catalyst, and utilizes capacitance material
Carry out the storage and release of light induced electron；
CNT and graphene are as a kind of super capacitor material, with prominent physicochemical properties, including good storage
Deposit electronic capability, excellent electric conductivity, ratio surface of super large etc..Therefore, can be with as the composition material of photochemical catalyst
Realize the storage of light induced electron；
The photochemical catalyst without metallic element that can be used under no light condition of the present invention is grey, internal presentation loose structure
Photochemical catalyst.By the first h of illumination 5 under xenon lamp of this photochemical catalyst, phenol is then selected as simulated environment pollutant, in nothing
Under conditions of illumination, it still can show that it still has certain catalytic activity under no light condition with the phenol in degradation water.
Claims (4)
1. a kind of photochemical catalyst without metallic element that can be used under no light condition, it is characterised in that：Described photocatalysis
Agent is made up of the raw material of following mass fraction：
The CNT 3-15 of functionalization
Graphene 1-5
Carbonitride 20-60.
2. a kind of side for preparing the photochemical catalyst without metallic element that can be used as claimed in claim 1 under no light condition
Method, it is characterised in that：Described method is followed the steps below：
CNT is put into the mixed liquor of 14.5mol/L concentrated nitric acid and the 18.4mol/L concentrated sulfuric acid first, and dense nitre
The volume ratio of acid and the concentrated sulfuric acid is 1:3, and mixed liquor is heated to 60-80 DEG C, and be incubated 2-6h, mixed liquor is carried out suction filtration or
Person's centrifugal treating, is washed out, up to neutral, obtaining the CNT of functionalization,
Then it is 3 the CNT of functionalization to be put into volume ratio:In 2 water and the mixed liquor of isopropanol, 2- is persistently stirred
6h, obtains carbon nano tube dispersion liquid, and ensures in carbon nano tube dispersion liquid, and the concentration of CNT is 9-18mg/mL, then
Graphene is added into carbon nano tube dispersion liquid, and 3-5h is persistently stirred on magnetic stirring apparatus, ultrasonically treated 2-4h, is obtained afterwards
Carbon nano tube/graphene dispersion liquid is obtained, carbonitride is put into carbon nano tube/graphene dispersion liquid, ultrasonically treated 1-5h is obtained
Whole dispersion liquid, by whole dispersion liquid under conditions of 140-180 DEG C hydro-thermal reaction 10-24h, then naturally cool to room temperature ,-
2-12h is freeze-dried under conditions of 50 to -20 DEG C, that is, obtains photochemical catalyst.
3. the photochemical catalyst without metallic element according to claim 1 that can be used under no light condition, its feature exists
In：Described graphene is graphene oxide or redox graphene.
4. the photochemical catalyst without metallic element according to claim 1 that can be used under no light condition, its feature exists
In：Described carbonitride is the carbonitride of nanocrystal monolayer or the carbonitride of nanometer multilayer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710229252.5A CN107008482A (en) | 2017-04-10 | 2017-04-10 | A kind of photochemical catalyst without metallic element that can be used under no light condition and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710229252.5A CN107008482A (en) | 2017-04-10 | 2017-04-10 | A kind of photochemical catalyst without metallic element that can be used under no light condition and preparation method thereof |
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| CN201710229252.5A Pending CN107008482A (en) | 2017-04-10 | 2017-04-10 | A kind of photochemical catalyst without metallic element that can be used under no light condition and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786892A (en) * | 2018-06-26 | 2018-11-13 | 江苏师范大学 | A kind of graphite oxide phase single layer C3N4Composite film material and its preparation method and application |
| CN111530488A (en) * | 2020-05-06 | 2020-08-14 | 江苏卓高环保科技有限公司 | Nano fiber matt catalytic microsphere and preparation method thereof |
| CN112023969A (en) * | 2020-08-20 | 2020-12-04 | 江苏大学 | 2D-g-C3N4Preparation method and application of/1D-MWNTs/2D-rGO hybrid photocatalytic material |
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| CN102989497A (en) * | 2012-12-07 | 2013-03-27 | 同济大学 | Mesoporous graphite type carbon nitride/nitrogen-doped graphene composite material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786892A (en) * | 2018-06-26 | 2018-11-13 | 江苏师范大学 | A kind of graphite oxide phase single layer C3N4Composite film material and its preparation method and application |
| CN108786892B (en) * | 2018-06-26 | 2020-12-22 | 江苏师范大学 | Graphite oxide phase single-layer C3N4Composite film material and preparation method and application thereof |
| CN111530488A (en) * | 2020-05-06 | 2020-08-14 | 江苏卓高环保科技有限公司 | Nano fiber matt catalytic microsphere and preparation method thereof |
| CN112023969A (en) * | 2020-08-20 | 2020-12-04 | 江苏大学 | 2D-g-C3N4Preparation method and application of/1D-MWNTs/2D-rGO hybrid photocatalytic material |
| CN112023969B (en) * | 2020-08-20 | 2023-06-13 | 江苏大学 | 2D-g-C 3 N 4 Preparation method and application of/1D-MWNTs/2D-rGO hybrid photocatalytic material |
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