CN107694605B - Carbon quantum dot@porphyryl metal organic framework catalyst and preparation method and application - Google Patents
Carbon quantum dot@porphyryl metal organic framework catalyst and preparation method and application Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000003054 catalyst Substances 0.000 title claims abstract description 25
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000001699 photocatalysis Effects 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000010531 catalytic reduction reaction Methods 0.000 claims abstract description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 9
- 239000013097 PCN-222 Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 6
- 239000005711 Benzoic acid Substances 0.000 claims description 5
- 235000010233 benzoic acid Nutrition 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 150000004032 porphyrins Chemical class 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 4
- 230000010757 Reduction Activity Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000008033 biological extinction Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000013032 photocatalytic reaction Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
Classifications
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- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
-
- B01J35/39—
-
- B01J35/61—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention belongs to new energy fields, and in particular to a kind of carbon quantum dot@porphyryl metal organic framework catalyst, and its preparation method and application.Metal-organic framework materials are to CO2There is good absorption property.And carbon quantum dot is to CO2There is good photo catalytic reduction activity.Using suitable means, absorption and photocatalysis are integrated into a kind of material, CO will be greatly improved2Photo catalytic reduction rate.We introduce carbon quantum dot in stable porous porphyryl metal-organic framework materials, by photocatalysis by CO2Efficiently it is reduced to the clean energy resource CO useful to the mankind.Catalyst in the present invention, while there is wide area extinction (ABSORPTION EDGE is more than 800nm) and CO absorption2Effect, the two synergistic effect has very high photo catalytic reduction activity.Catalyst in the present invention has good chemical stability and thermal stability.Synthesis technology process of the present invention is simple, and strong operability has broad application prospects.
Description
Technical field
The invention belongs to new energy fields, and in particular to carbon quantum dot@porphyryl metal organic framework catalyst, and its system
Preparation Method and application.
Background technique
Most scientist thinks high concentration CO2Lead to greenhouse effects, so that Global Temperature increases, disruption of ecological balance.And by CO2
Capture utilizes, and being converted into cleaning new energy is that scientists want always the project captured.
Metal-organic framework materials, as a kind of emerging tool high porosity, high-specific surface area, adjustable structure and function
Porous material, gas absorption separation, small molecule detection and in terms of had some applications.Carbon quantum dot (CQD) because
Its hypotoxicity, biocompatibility, chemical inertness, low price, fluorescence and have simultaneously electron and receive electronics ability and
The concern of a large number of researchers is attracted.
Metal-organic framework materials are to CO2There is good absorption property, and carbon quantum dot is to CO2There is good photocatalysis also
Former activity.And suitable means are used, absorption and photocatalysis are integrated into a kind of material, CO will be greatly improved2Photocatalysis
Rate of reduction.
In order to solve the above problem, we introduce carbon quantum dot in stable porous porphyryl metal-organic framework materials,
By photocatalysis by CO2Efficiently it is reduced to the clean energy resource CO useful to the mankind.
Summary of the invention
The present invention is exactly to provide one kind in order to overcome the defects of the prior art described above and have both quick adsorption performance, bloom
The preparation method and application of the porous catalyst of catalytic activity, high chemical and thermal stability.
The purpose of the present invention can be achieved through the following technical solutions:
By the method for " from bottom to top ", or pass through the method for " from top to bottom ", obtains carbon quantum dot, it is preferable that pass through
Graphite rod is electrolysed by method " from top to bottom ", obtains carbon quantum dot.Then carbon quantum dot confinement is arrived with " bottle is around ship method "
In the duct of porphyryl metal organic framework, it is preferable that use " bottle is around ship method " by the duct of carbon quantum dot confinement to PCN-222
In, the specific steps are as follows:
(1) preparation of carbon quantum dot: being added deionized water in beaker, and two graphite electrodes are put into above-mentioned beaker,
And logical 15~90V direct current, after electrolysis 1~30 day, limpid colourless water becomes the aqueous solution of brownish black.By the black aqueous solution
After being filtered with filter paper, it is centrifuged 5 minutes to 2 hours with 10000 rpms or more of speed, and take supernatant.Supernatant is passed through
Drying is rotated, the carbon quantum dot of needs is obtained.
(2) the DEF solution preparation of carbon quantum dot:
It takes carbon quantum dot to be added in DEF, obtains the solution of 5mg/mL.
(3) preparation of carbon quantum dot@PCN-222:
By zirconium chloride (50~90mg), DEF (4~12mL), the DEF solution (0~1000 μ L) of carbon quantum dot, four (p-
Carboxylic acid phenyl) porphyrin (30~50mg) and benzoic acid (2-5g) are uniformly mixed, and 24~100 are kept the temperature in 110~140 DEG C of baking ovens
Hour, obtained solid washs 1~6 time through DMF.Then obtained solid is added in 100mL autoclave, and is added wherein
Enter the DMF solvent and 0.1~1.5mL concentrated hydrochloric acid of 12mL, 120 DEG C keep the temperature 6~24 hours.Then centrifugation removes supernatant, and adds
Enter acetone, every other day change an acetone, replaces 1~6 time, obtain solid powder.
In the present invention, catalyst made from the method is used to photo catalytic reduction CO2。
In the present invention, photo catalytic reduction CO2The step of be: take 10mg carbon quantum dot@PCN-222 catalyst to be dispersed in
On quartzy filter membrane, be placed in solid gas photocatalytic reaction device, be added 0~5mL acetonitrile and triethanolamine mixed liquor (acetonitrile with
Triethanolamine volume ratio is 1~10:1), it is vacuumized at 1~6 time and fills CO2Afterwards, making reaction, balance 0~5 is small in a dark environment
When.Then, reaction unit is placed under visible lamp, every the CO concentration of survey in 0.1~4 hour.
Compared with prior art, the invention has the following advantages that
1, the catalyst in the present invention, while there is wide area extinction (ABSORPTION EDGE is more than 800nm) and CO absorption2Effect,
The two synergistic effect has very high photo catalytic reduction activity.
2, the catalyst in the present invention has very high specific surface area, can a large amount of CO absorptions2, promote photocatalytic activity.
3, the catalyst in the present invention has good chemical stability and thermal stability.
4, synthesis technology process of the present invention is simple, and strong operability has broad application prospects.
Detailed description of the invention
Fig. 1 is carbon quantum dot@PCN-222 prepared by embodiment 1, the transmission electron microscope picture after decomposing.
Fig. 2 is the powder XRD pattern of carbon quantum dot@PCN-222 prepared by embodiment 1.
Fig. 3 is the nitrogen adsorption isotherm of carbon quantum dot@PCN-222 prepared by embodiment 1.
Fig. 4 is catalyst carbon quantum dot the@PCN-222 and PCN-222 of the preparation of embodiment 1 to CO2Photo catalytic reduction effect
Fruit figure.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
(1) preparation of carbon quantum dot:
500mL deionized water is added in the beaker of 500mL, two Graphene electrodes are put into above-mentioned beaker, spacing
7cm, and logical 30V direct current, after two weeks, limpid colourless water becomes the aqueous solution of black for electrolysis.The black aqueous solution is filtered
After paper filtering, it is centrifuged one hour with 20000 rpms of speed, and take supernatant.By supernatant through rotating drying, must need
Carbon quantum dot.
(2) the DEF solution preparation of carbon quantum dot:
It takes 25mg GQDs to be added in 5mLDEF, obtains the GQDs/DEF solution of 5mg/mL.
(3) preparation of carbon quantum dot@PCN-222:
By zirconium chloride (70mg), DEF (8mL), the DEF solution (200 μ L) of carbon quantum dot, four (p- carboxylic acid phenyl) porphins
Quinoline (50mg) and benzoic acid (2.7g) are uniformly mixed, and keep the temperature 48 hours in 120 DEG C of baking ovens, and it is small that 24 are kept the temperature in 130 DEG C of baking ovens
When, obtained solid washs four times through DMF.Then obtained solid is added in 100mL autoclave, and is added wherein
The DMF solvent and 1.5mL concentrated hydrochloric acid of 12mL, 120 DEG C keep the temperature 12 hours.Then centrifugation removes supernatant, and acetone is added, often
An acetone is changed every two days, and displacement three times, obtains solid powder.
(4) preparation of comparative catalyst PCN-222: by zirconium chloride (70mg), DEF (8mL), four (p- carboxylic acid phenyls)
Porphyrin (50mg) and benzoic acid (2.7g) are uniformly mixed, and keep the temperature 48 hours in 120 DEG C of baking ovens, keep the temperature 24 in 130 DEG C of baking ovens
Hour, obtained solid washs four times through DMF.Then obtained solid is added in 100mL autoclave, and is added wherein
The DMF solvent and 1.5mL concentrated hydrochloric acid of 12mL, 120 DEG C keep the temperature 12 hours.Then centrifugation removes supernatant, and acetone is added, often
An acetone is changed every two days, and displacement three times, obtains solid powder.
The object phase of catalyst carbon quantum dot@PCN-222 and PCN-222 are characterized by powder X-ray RD.Pass through nitrogen adsorption isothermal
Line shows that catalyst has very big specific surface area and porosity, is conducive to the mass transport process during subsequent catalyst.
Embodiment 2:
Carbon quantum dot@PCN-222 catalyst photo catalytic reduction CO2Performance evaluation: take 10mgGQDs@PCN-222 be catalyzed
Agent is dispersed on quartzy filter membrane, is placed in solid gas photocatalytic reaction device, and the mixing of 2mL acetonitrile and triethanolamine is added
Liquid (acetonitrile is 4:1 with triethanolamine volume ratio), fills CO vacuumizing three times2Afterwards, making reaction, balance 1 is small in a dark environment
When.Then, reaction unit is placed under 300W visible lamp, every the CO concentration of survey in two hours.
Embodiment 3:
Comparative catalyst PCN-222 photo catalytic reduction CO2Performance evaluation: take 10mg PCN-222 catalyst evenly dispersed
On quartzy filter membrane, be placed in solid gas photocatalytic reaction device, be added 2mL acetonitrile and triethanolamine mixed liquor (acetonitrile with
Triethanolamine volume ratio is 4:1), CO is filled vacuumizing three times2Afterwards, reaction is balanced 1 hour in a dark environment.Then, will
Reaction unit is placed under 300W visible lamp, every the CO concentration of survey in two hours.
The description of above-described embodiment is for convenience of that can understand and apply the invention in those skilled in the art.
Those skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments, without passing through creative work.Therefore, the present invention is not limited to embodiments here.
Those skilled in that art according to the present invention, to the improvement made of the present invention and modification all should protection scope of the present invention it
It is interior.
Claims (3)
1. carbon quantum dot@porphyryl metal organic framework catalyst；Wherein carbon quantum dot is by the method for " from top to bottom " by stone
Inker is electrolysed in deionized water；Wherein porphyryl metal organic framework is PCN-222；Wherein catalyst is carbon quantum dot@
PCN-222；Wherein the preparation method of carbon quantum dot@porphyryl metal organic framework catalyst is to use " bottle is around ship method " by carbon amounts
Son puts confinement into the duct of PCN-222, specifically: by zirconium chloride, DEF, the DEF solution of carbon quantum dot, four (p- carboxylic acids
Phenyl) porphyrin and benzoic acid be uniformly mixed, and 110 ~ 140o24 ~ 100 hours are kept the temperature in C baking oven, obtained solid is washed through DMF
It washs 1 ~ 6 time；Then by obtained solid be added 100mL autoclave in, and wherein be added 12mL DMF solvent and 0.1 ~
1.5mL concentrated hydrochloric acid, 120oC keeps the temperature 6 ~ 24 hours；Then centrifugation removes supernatant, and acetone is added, and every other day changes one time third
Ketone replaces 1 ~ 6 time, obtains solid powder.
2. a kind of preparation method of carbon quantum dot@porphyryl metal organic framework catalyst described in claim 1, feature exist
In as follows: zirconium chloride, DEF, the DEF solution of carbon quantum dot, four (p- carboxylic acid phenyl) porphyrins and benzoic acid are uniformly mixed,
And 110 ~ 140o24 ~ 100 hours are kept the temperature in C baking oven, obtained solid washs 1 ~ 6 time through DMF；Then obtained solid is added
In 100mL autoclave, and wherein be added 12mL DMF solvent and 0.1 ~ 1.5mL concentrated hydrochloric acid, 120oC heat preservation 6 ~ 24 is small
When；Then centrifugation removes supernatant, and acetone is added, and every other day changes an acetone, replaces 1 ~ 6 time, obtains solid powder.
3. a kind of carbon quantum dot@porphyryl metal organic framework catalyst described in claim 1 is used for photo catalytic reduction CO2。
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| CN108686705A (en) * | 2018-05-04 | 2018-10-23 | 大连理工大学 | A kind of carbon quantum dot-ZIF-67 absorption-photochemical catalyst and preparation method thereof |
| CN109464986A (en) * | 2018-11-29 | 2019-03-15 | 西北师范大学 | A kind of preparation and application of the nanocomposite based on porphyrin metal organic frame and ternary sulfide |
| CN111420654B (en) * | 2019-01-09 | 2021-06-22 | 中国科学院福建物质结构研究所 | Carbon-based nano material and preparation method and application thereof |
| CN110551318B (en) * | 2019-08-12 | 2021-12-03 | 上海利物盛纳米科技有限公司 | Preparation method of graphene-based heat and moisture exchange composite membrane |
| CN111129512B (en) * | 2019-12-27 | 2021-09-14 | 大连理工大学 | Nano carambola-shaped oxygen reduction electrocatalyst and preparation method and application thereof |
| CN111659455B (en) * | 2020-07-29 | 2022-08-26 | 重庆工商大学 | Preparation method and application of Co-CDs @ NM photocatalyst |
| CN113244962B (en) * | 2021-05-24 | 2022-11-01 | 常州大学 | Preparation method and application of singlet oxygen generating zirconium porphyrin-based MOF-graphene composite photocatalyst |
| CN114016075B (en) * | 2021-11-12 | 2023-09-15 | 上海大学 | High-selectivity CO 2 Preparation method and application of electrocatalytic reduction CO carbon quantum dot catalyst |
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| CN106010540B (en) * | 2016-05-11 | 2018-02-16 | 中国科学院福建物质结构研究所 | A kind of quantum dot/metal organic framework laminated film and its preparation and application |
| CN106215979A (en) * | 2016-07-07 | 2016-12-14 | 中国科学院福建物质结构研究所 | The preparation of load-type iron-based metallic organic framework oxidation-desulfurizing catalyst and application thereof |
| CN106252676B (en) * | 2016-07-28 | 2018-05-11 | 青岛大学 | A kind of preparation of quantum dot modified metal organic backbone insertion carbon nano-tube material |
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| CN106947475B (en) * | 2017-03-30 | 2020-01-10 | 皖西学院 | Preparation method of fluorescent carbon quantum dots and detection of Al in water by using fluorescent carbon quantum dots3+Ion application |
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