CN106334572A - Cu/Co@NPC compound used for catalytic reduction of p-nitrophenol - Google Patents
Cu/Co@NPC compound used for catalytic reduction of p-nitrophenol Download PDFInfo
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- CN106334572A CN106334572A CN201610609790.2A CN201610609790A CN106334572A CN 106334572 A CN106334572 A CN 106334572A CN 201610609790 A CN201610609790 A CN 201610609790A CN 106334572 A CN106334572 A CN 106334572A
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- 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
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Abstract
The invention relates to a nitrogen modified carbon (NPC) coated copper/cobalt (Cu/Co@NPC) compound obtained through a roasting technology with Cu-Co Prussian blue Cu3<II>[Co<III>(CN)6]2(Cu-Co PBA) as a template. A preparation method of the compound comprises the following steps: synthesizing Cu-Co PBA through a standing technology, and roasting the Cu-Co PBA in a tubular furnace in Ar/N2 atmosphere at different temperatures to obtain the Cu/Co@NPC compound.
Description
Technical field
Present invention cu-co Prussian blue analogue cuii 3[coiii(cn)6]2(cu-co pba) is having of templated synthesis
Copper cobalt (the cu/co@npc) compound that the charcoal bag of high-specific surface area and the modification of ferromagnetic nitrogen is covered, can be as reduction to nitro
The catalyst of phenol.
Background technology
Para-aminophenol (pap) is a kind of important chemical industry and medicine intermediate, is mainly used in synthesis antipyretic-antalgic
The aspects such as medicine, rubber chemicals, dyestuff, feed, petroleum additive and photographic developer.China produces pap mainly using right at present
Nitrophenol (pnp) iron powder reducing method and pnp catalytic hydrogenation method.Iron powder reducing method production cost is high, seriously polluted；Catalysis adds
Hydrogen method process is simple, good product purity, but pd type catalyst is expensive, ni type catalyst easy in inactivation.Therefore, research and develop low one-tenth
Originally the environmentally friendly non-precious metal catalyst that, catalytic performance is excellent, preparation condition is gentle has important practical significance.Transition
Metal and its compound enriched due to its low cost, reserves, environmentally friendly the features such as, by a lot of as catalyst research.
Wherein Nanometer Copper (cu), nanometer cobalt (co) have the advantages that catalysis activity is high, are given a lot of concerns.
Nano-cu, co catalysis activity high, cheap, environmentally friendly, be a kind of preferable heterogeneous catalysis.General
Logical nano-cu, co easily reunite, and catalytic performance is poor.The cu/co@npc being obtained for template roasting with cu-co pba is hence it is evident that improve
Common nano-cu, the agglomeration of co, improve Catalytic Hydrogenation Properties, and cu, the co inactivating is easy to regenerate, and is easy to reality
Application.
The present invention has the cu/co@npc compound of very high-specific surface area with cu-co pba for templated synthesis.The method
Have the advantages that reaction condition is gentle, simple.
Content of the invention
It is templated synthesis cu/co@npc compound that this experiment is provided with cu-co pba.Operating procedure is as follows:
(1) in aqueous systems, sodium citrate (na3c6h5o7·2h2O), potassium citrate (k3c6h5o7·h2O) it is yardstick adjusting control agent,
Copper nitrate (cu (no3)2·3h2O), copper chloride (cucl2·2h2O), copper sulphate (cuso4·5h2O), copper acetate (cu
(ch3coo)2·h2O) respectively with potassium hexacyanocobaltate (k3[co(cn)6]), six cyanogen close cobalts acid sodium (na3[co(cn)6]) anti-
Should, generate cu-co pba.
(2) in 600-800oC, argon gas/nitrogen (ar/n2) atmosphere roasting cu-co pba obtain cu/co@npc be combined
Thing.
Brief description
Fig. 1 is cu/co@npc compound scanning electron microscope (SEM) photograph.
Fig. 2 is cu/co@npc compound transmission electron microscope picture.
Fig. 3 is the ultraviolet-visible spectrogram that cu/co npc complex catalysts reduce p-nitrophenol.
Fig. 4 is the performance impact figure to catalysis reduction p-nitrophenol for the cu/co@npc compound consumption.
Fig. 5 is the performance impact figure that cu/co@npc complex catalysts reduce p-nitrophenol.
Specific embodiment
By specific embodiment, the present invention is explained in further detail:
Embodiment 1:0.6 mmol cu (no3)2·3h2o、0.9 mmol na3c6h5o7·2h2O is dissolved in 15 ml deionizations
In water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly, room
Aging 24 h under temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC vacuum is done
Dry.Dried pressed powder is in tube furnace ar atmosphere 600oC roasting 3 h, heating rate is 2oc·min-1, referring to accompanying drawing
1 to accompanying drawing 5.
Embodiment 2:0.6 mmol cucl2·2h2o、0.9 mmol na3c6h5o7·2h2O be dissolved in 15 ml go from
In sub- water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly,
Aging 24 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC vacuum
It is dried.Dried pressed powder is in tube furnace ar atmosphere 600oC roasting 3 h, heating rate is 2oc·min-1.
Embodiment 3:0.6 mmol cuso4·5h2o、0.9 mmol na3c6h5o7·2h2O be dissolved in 15 ml go from
In sub- water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly,
Aging 24 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC vacuum
It is dried.Dried pressed powder is in tube furnace ar atmosphere 600oC roasting 3 h, heating rate is 2oc·min-1.
Embodiment 4:0.6 mmol cu (ch3coo)2·h2o、0.9 mmol na3c6h5o7·2h2O is dissolved in 15 ml
In deionized water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, will be rapid for above two solution
Mixing, aging 24 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oc
Vacuum drying.Dried pressed powder is in tube furnace ar atmosphere 600oC roasting 3 h, heating rate is 2oc·min-1.
Embodiment 5:0.6 mmol cu (no3)2·3h2o、0.9 mmol k3c6h5o7·h2O be dissolved in 15 ml go from
In sub- water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly,
Aging 24 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC vacuum
It is dried.Dried pressed powder is in tube furnace ar atmosphere 600oC roasting 3 h, heating rate is 2oc·min-1.
Embodiment 6:0.6 mmol cu (no3)2·3h2o、0.9 mmol na3c6h5o7·2h2O is dissolved in 15 ml and goes
In ionized water, separately take 0.4 mmol na3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly
Close, aging 36 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC is true
Empty dry.Dried pressed powder is in tube furnace ar atmosphere 600oC roasting 3 h, heating rate is 2oc·min-1.
Embodiment 7:0.6 mmol cu (no3)2·3h2o、0.9 mmol na3c6h5o7·2h2O is dissolved in 15 ml and goes
In ionized water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly
Close, aging 24 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC is true
Empty dry.Dried pressed powder is in tube furnace n2Atmosphere 600oC roasting 3 h, heating rate is 2oc·min-1.
Embodiment 8:1.2 mmol cu (no3)2·3h2o、1.8 mmol na3c6h5o7·2h2O is dissolved in 15 ml and goes
In ionized water, separately take 0.8 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly
Close, aging 48 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC is true
Empty dry.Dried pressed powder is in tube furnace ar atmosphere 600oC roasting 3 h, heating rate is 2oc·min-1.
Embodiment 9:0.6 mmol cu (no3)2·3h2o、0.9 mmol na3c6h5o7·2h2O is dissolved in 15 ml and goes
In ionized water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly
Close, aging 24 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC is true
Empty dry.Dried pressed powder is in tube furnace ar atmosphere 700oC roasting 3 h, heating rate is 2oc·min-1, referring to
Accompanying drawing 5.
Embodiment 10:0.6 mmol cu (no3)2·3h2o、0.9 mmol na3c6h5o7·2h2O is dissolved in 15 ml and goes
In ionized water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly
Close, aging 24 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC is true
Empty dry.Dried pressed powder is in tube furnace ar atmosphere 800oC roasting 3 h, heating rate is 2oc·min-1, referring to
Accompanying drawing 5.
Embodiment 11:0.6 mmol cu (no3)2·3h2o、0.9 mmol na3c6h5o7·2h2O is dissolved in 15 ml and goes
In ionized water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly
Close, aging 24 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC is true
Empty dry.Dried pressed powder is in tube furnace ar atmosphere 800oC roasting 6 h, heating rate is 2oc·min-1.
Embodiment 12:0.6 mmol cu (no3)2·3h2o、0.9 mmol na3c6h5o7·2h2O is dissolved in 15 ml and goes
In ionized water, separately take 0.4 mmol k3[co(cn)6] be dissolved in 15 ml deionized waters, above two solution is mixed rapidly
Close, aging 24 h under room temperature.It is centrifuged to obtain pressed powder, wash several times respectively by deionized water and ethanol for this pressed powder, 60oC is true
Empty dry.Dried pressed powder is in tube furnace ar atmosphere 600oC roasting 6 h, heating rate is 8oc·min-1.
Claims (4)
1. one kind is with cu-co Prussian blue analogue cuii 3[coiii(cn)6]2(cu-co pba) is template, high-temperature roasting synthetic nitrogen
Copper cobalt (the cu/co@npc) compound that the charcoal (npc) modified coats, has and for p-nitrophenol to be reduced to para-aminophenol
Catalytic performance.
2. according to claim 1 it is characterised in that: in cu-co pba, copper nitrate (cu (no3)2·3h2O), chlorination
Copper (cucl2·2h2O), copper sulphate (cuso4·5h2O), copper acetate (cu (ch3coo)2·h2O) it is cuiiBody, six cyanogen are provided
Close cobalt acid potassium (k3[co(cn)6]), six cyanogen close cobalts acid sodium (na3[co(cn)6]) it is coiiiBody is provided.
3. according to claim 1 it is characterised in that: sodium citrate (na3c6h5o7·2h2O), potassium citrate (k3c6h5o7·
h2O) it is cu-co pba yardstick adjusting control agent.
4. according to claim 1 it is characterised in that: in 600-800oC, argon gas/nitrogen (ar/n2) in roasting obtain cu/
Co@npc compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610609790.2A CN106334572A (en) | 2016-07-28 | 2016-07-28 | Cu/Co@NPC compound used for catalytic reduction of p-nitrophenol |
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| CN201610609790.2A CN106334572A (en) | 2016-07-28 | 2016-07-28 | Cu/Co@NPC compound used for catalytic reduction of p-nitrophenol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106881141A (en) * | 2017-04-19 | 2017-06-23 | 福州大学 | Cobalt/hexagonal boron nitride complex nucleus shell structural nano catalyst and its preparation and application |
| CN112378968A (en) * | 2020-11-09 | 2021-02-19 | 安徽工业大学 | Sensor for hydrazine detection, nitrogen-doped porous carbon-loaded copper-cobalt nanocomposite material, and preparation method and application thereof |
| CN116334686A (en) * | 2023-05-29 | 2023-06-27 | 中石油深圳新能源研究院有限公司 | Ruthenium nitrogen doped carbon coated copper-cobalt alloy nano-catalyst and preparation method thereof |
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| CN102437324A (en) * | 2011-12-12 | 2012-05-02 | 中国科学技术大学 | Preparation method of cobalt-manganese composite oxide nanoparticles and cobalt-manganese composite oxide nanoparticles prepared by adopting same |
| CN103752321A (en) * | 2014-01-02 | 2014-04-30 | 上海大学 | Method for preparing hierarchical bimetallic composite oxide denitrification catalyst |
| CN104282908A (en) * | 2014-09-24 | 2015-01-14 | 张五星 | Method for synthesizing high-sodium iron-based Prussian blue electrode material |
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2016
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Patent Citations (3)
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| CN102437324A (en) * | 2011-12-12 | 2012-05-02 | 中国科学技术大学 | Preparation method of cobalt-manganese composite oxide nanoparticles and cobalt-manganese composite oxide nanoparticles prepared by adopting same |
| CN103752321A (en) * | 2014-01-02 | 2014-04-30 | 上海大学 | Method for preparing hierarchical bimetallic composite oxide denitrification catalyst |
| CN104282908A (en) * | 2014-09-24 | 2015-01-14 | 张五星 | Method for synthesizing high-sodium iron-based Prussian blue electrode material |
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| JAKKID SANETUNTIKUL ET AL.: "Prussian Blue-Carbon Hybrid as a Non-Precious Electrocatalyst for the Oxygen Reduction Reaction in Alkaline Medium", 《ELECTROCHIMICA ACTA》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106881141A (en) * | 2017-04-19 | 2017-06-23 | 福州大学 | Cobalt/hexagonal boron nitride complex nucleus shell structural nano catalyst and its preparation and application |
| CN106881141B (en) * | 2017-04-19 | 2019-09-13 | 福州大学 | Cobalt/hexagonal boron nitride complex nucleus shell structural nano catalyst and its preparation and application |
| CN112378968A (en) * | 2020-11-09 | 2021-02-19 | 安徽工业大学 | Sensor for hydrazine detection, nitrogen-doped porous carbon-loaded copper-cobalt nanocomposite material, and preparation method and application thereof |
| CN112378968B (en) * | 2020-11-09 | 2023-08-22 | 安徽工业大学 | Sensor for hydrazine detection, nitrogen-doped porous carbon-loaded copper-cobalt nanocomposite and preparation method and application thereof |
| CN116334686A (en) * | 2023-05-29 | 2023-06-27 | 中石油深圳新能源研究院有限公司 | Ruthenium nitrogen doped carbon coated copper-cobalt alloy nano-catalyst and preparation method thereof |
| CN116334686B (en) * | 2023-05-29 | 2023-07-28 | 中石油深圳新能源研究院有限公司 | Ruthenium nitrogen doped carbon coated copper-cobalt alloy nano-catalyst and preparation method thereof |
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Application publication date: 20170118 |