CN107597143A - A kind of metal nanoparticle is uniformly embedded into the controllable method for preparing of the elctro-catalyst of mesoporous carbon spheres internal structure - Google Patents
A kind of metal nanoparticle is uniformly embedded into the controllable method for preparing of the elctro-catalyst of mesoporous carbon spheres internal structure Download PDFInfo
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Abstract
The controllable method for preparing of the elctro-catalyst of mesoporous carbon spheres internal structure is uniformly embedded into the invention discloses a kind of metal nanoparticle, it is characterised in that configure phenol, formaldehyde, the mixed liquor of melamine in proportion, reacted；F127 is added in reaction mixture to continue to react；In mixed solution system, water is added, makes its reaction overnight；Reaction solution is mixed with deionized water, then adds metal precursor powder, then adjust the pH value of mixed liquor；Hydro-thermal in water heating kettle is put into after mixed liquor is stirred；After product after hydro-thermal is centrifuged successively, washed, is dried, calcining, obtaining uniform load has the noble metal@mesoporous carbon spheres of different-grain diameter size, i.e. Pd [email protected] preparation method technique is simple, and cost is relatively low, and obtained mesoporous carbon spheres particle size is controllable and homogeneous, surface area is big, and catalyst component good dispersion, electric conductivity is preferable, and catalytic activity is high, and generation nitrogen selective is high, and stability is good, can repeatedly use.
Description
Technical field
The invention belongs to the nitrate removal technical field in water body, it is related to that a kind of particle size is adjustable, is uniformly embedded with
The controlledly synthesis preparation method of the mesoporous carbon spheres elctro-catalyst of noble metal nano particles.
Background technology
The irrational industrial Agricultural Activities of modern society, make underground water pollution environment be increasingly becoming global world's model
Interior new significant problem is enclosed, and nitrate anion, due to stability high in aqueous, it largely enters lake, river mouth, bay
Etc. slow fluid, the rapid breeding of algae and other planktonic organisms can be caused, dissolved oxygen in water declines, and fish and other biologies are big
Dead phenomenon is measured, and then makes water quality deterioration.Nitrate concentration increase can cause to seriously endanger to human health in drinking-water, work as people
When body injects excessive nitrate, except a part is discharged by kidney, unnecessary is then converted into nitrous acid by digestive system
Salt is combined with hemoglobin, and blood is lost blood transfusion ability causes blood anoxic, so that adult suffers from methemoglobinemia.
At present, azotate pollution has been a fairly common global environmental problem in underground water.Most of areas are used as drinking water
The underground water in source is polluted by nitrate to some extent, and has the trend aggravated year by year, in indivedual regional underground water
The concentration of nitrate is more than 100mg/L.Originally individual water shortage country of China, water resource is only the four of world's quantity per capita per capita
/ mono-, for one of country of most water shortage in the world.And this few water resource will also meet the industrial and agricultural production of high speed development
Demand, the result is that original extremely rare domestic water because the pollution of production and living becomes more rare,
In China, protection and treating groundwater are particularly important to economy and social effect.
In recent years in order to convert and thoroughly remove nitrate excessive in water body, various water process is developed and has taken off
Nitrogen technology：Physical chemistry denitrogenation (ion-exchange, hyperfiltration, electroosmose process), biological denitrificaion method (denitrifying bacteria generation
Thank), catalytic reduction denitrogenation method (photocatalysis, liquid phase catalytic reduction, electro-catalysis).The expense of physico-chemical process is not low, efficiency not
Height, denitrification effect in by water body many factors influenceed, and actually not thoroughly remove nitrate pollutants, be into
Simple transfer and concentration are gone, the sewage disposal for high concentration, complicated component is difficult to apply.Biological denitrificaion method is exactly to utilize
Reducing nitrate radical is gaseous nitrogen by denitrifying bacteria, and it not only needs acclimated microorganism, and is needed to build and be adapted to its growth
Environment.It is ammonia nitrogen that photo catalytic reduction, which removes most of product that nitrate anion obtains, and quantum utilization rate is low, it is necessary to adds hole agent
Reactivity can be improved.Liquid phase catalytic reduction method is mainly using hydrogen as reducing agent, directly by nitrate anion in the presence of catalyst
Ion conversion is nitrogen, but solubility of the hydrogen under common water quality and water temperature condition is small, is unfavorable for the reality of catalytic reduction
Apply on border.
Electro-catalysis reducing process is very promising sewage disposal that is a kind of while meeting security and cost-effectiveness requirement
Technology.Nitrate anion in water is thoroughly reduced to other nitrogenous class innocuous substances by it, and need not add reducing agent, will not be caused
Without subsequent treatment, reactor is simple, automaticity is high is adapted to large-scale application for secondary pollution and reaction water outlet.Electro-catalysis
Have the advantages that the high multicomponent energy consumption of selectivity is low and security, it is turned into researcher's focus of attention in recent years.
Electro catalytic electrode includes active component and carrier two parts, and catalytic active component is also from one-component to double groups in recent years
Part even trend of multicomponent development, wherein metal material such as Cu, Fe, Ni, Pt, Pd, Sn etc. are used as nitrate in water body
The catalytic active component of electro-catalysis reduction, these active components and different combinations have different catalytic activity and gas choosing
Selecting property.Carrier generally has carbon, graphite, metal etc., and it cuts both ways, and as electric conductivity is not good enough, reaction surface area is not big enough, activity
The scattered uneven easily reunion of component, active component easily depart from loss etc. on surface.Therefore suitable active component and carrier are selected
Combination Design, it is particularly important to improving catalytic activity.
The content of the invention
Problem to be solved by this invention is：There is provided that a kind of particle size, noble metal species are controllable, and inner homogeneous is embedding
There is the controlledly synthesis preparation method of the mesoporous carbon spheres elctro-catalyst of noble metal nano particles.
In order to solve the above problems, the present invention uses following technical scheme：A kind of metal nanoparticle is uniformly embedded into mesoporous
The controllable method for preparing of the elctro-catalyst of carbon ball internal structure, it is characterised in that comprise the following steps that：
Step 1)：Phenol, formaldehyde, the mixed liquor of melamine are configured in proportion, are reacted；
Step 2)：F127 is added in reaction mixture made from step 1) to continue to react；
Step 3)：In mixed solution system made from step 2), water is added, makes its reaction overnight；
Step 4)：Reaction solution made from step 3) is mixed with deionized water, then adds metal precursor powder, then adjust
Save the pH value of mixed liquor；
Step 5)：Hydro-thermal in water heating kettle is put into after mixed liquor made from step 4) is stirred；
Step 6)：Product after the hydro-thermal that step 5) is obtained centrifuged, washed, being dried successively, calcine after, obtain
The even noble metal@mesoporous carbon spheres for being loaded with different-grain diameter size, i.e. Pd-Cu@mCS.
Preferably, the mol ratio of phenol and formaldehyde is 5: 1~1: 5 in the step 1)；Mole of formaldehyde and melamine
Than for 100: 0~1: 20；Reaction condition is：At 40~100 DEG C, 10~300min is reacted.
Preferably, F127 addition is the 0.1~30% of reaction mixture quality in the step 2)；Reaction time
2~3h.
Preferably, the addition of the step 3) reclaimed water is the 0.1~30% of reaction mixture volume；Reaction time is
6~30h.
Preferably, the volume ratio of reaction solution and deionized water is 1: 1~1: 200 in the step 4)；Metal precursor powder
Last palladium using gold and its compound, platinum and its compound, ruthenium and its compound, copper and its compound, Cobalt and compounds of cobalt, iron and
Any one or a few composition in its compound and sodium and its compound；PH values are adjusted to 8~12.
It is highly preferred that the metal precursor powder is using palladium sodium chlorate and the mixture of nitrate trihydrate copper, palladium sodium chlorate
Mol ratio with nitrate trihydrate copper is 1: 4~4: 1.
Preferably, the temperature of hydro-thermal is 80~180 DEG C in the step 5), and the hydro-thermal time is 2-24h.
Preferably, the atmosphere of calcining be argon hydrogen gaseous mixture in the step 6), and calcining heat is 300~900 DEG C, during calcining
Between be 2~8h.
Preferably, the Pd-Cu in the Pd-Cu@mCS that the step 6) obtains exists in the form of alloy.
Preferably, the pore-size distribution for the Pd-Cu@mCS that the step 6) obtains is 1.9~4.4nm, specific surface area 540
~570m2/ g, pore volume scope are 0.3~0.5cm3/g。
Compared with prior art, the beneficial effects of the present invention are：It is used for denitrogenation in water body the invention provides a kind of
The preparation method of elctro-catalyst Pd-Cu@mCS balls.The preparation method technique is simple, and cost is relatively low, obtained mesoporous carbon spheres particle diameter
Size is controllable and homogeneous, surface area is big, and catalyst component good dispersion, electric conductivity is preferable, and catalytic activity is high, generates nitrogen selective
Height, stability is good, can repeatedly use.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture (abbreviation TEM figures) of obtained elctro-catalyst in embodiment 1；
Fig. 2 is the transmission electron microscope picture (abbreviation TEM figures) of obtained elctro-catalyst in embodiment 2；
Fig. 3 is the transmission electron microscope picture (abbreviation TEM figures) of obtained elctro-catalyst in embodiment 3.
Embodiment
To become apparent the present invention, hereby with preferred embodiment, and accompanying drawing is coordinated to be described in detail below.
Embodiment 1
A kind of metal nanoparticle is uniformly embedded into the controllable method for preparing of the elctro-catalyst of mesoporous carbon spheres internal structure：
(1) phenol: formaldehyde: melamine=4: the mixed liquor of 13: 1 mol ratios is configured；
(2) after reaction mixture is reacting 30 minutes for 65 DEG C in (1), the mass fraction for adding F127 is 4%；
(3) when in (2) mixed solution system continue to react 2 hours at 65 DEG C, the rear deionized water for adding 50mL, make its anti-
Answer 16 hours；
(4) reaction solution in (3) is mixed with deionized water volume with 4: 1, add palladium, copper precursor powder be respectively 1mg,
3mg, after pH of mixed is adjusted to 9.5；
(5) hydro-thermal 24 hours at 130 DEG C are respectively put into water heating kettle after mixed liquor in (4) is stirred；
(6) the obtained product after (5) hydro-thermal centrifuged, washed, after drying, 700 DEG C under argon hydrogen mixed atmosphere
Lower calcining 3 hours, then obtains metal@mesoporous carbon spheres (Pd-Cu@mCS).
Fig. 1 is that the TEM of catalyst made from the present embodiment schemes, and the dash area in figure is the ground gold of embedded mesoporous carbon spheres
Metal particles.
Embodiment 2
A kind of metal nanoparticle is uniformly embedded into the controllable method for preparing of the elctro-catalyst of mesoporous carbon spheres internal structure：
(1) phenol: formaldehyde: melamine=4: the mixed liquor of 13: 1 mol ratios is configured；
(2) after reaction mixture is reacting 30 minutes for 65 DEG C in (1), the mass fraction for adding F127 is 4%；
(3) when in (2) mixed solution system continue to react 2 hours at 65 DEG C, the rear deionized water for adding 50mL, make its anti-
Answer 16 hours；
(4) reaction solution in (3) is mixed with deionized water volume with 3: 1, add palladium, copper precursor powder be respectively 1mg,
3mg, after pH of mixed is adjusted to 9.5；
(5) hydro-thermal 24 hours at 130 DEG C are respectively put into water heating kettle after mixed liquor in (4) is stirred；
(6) the obtained product after (5) hydro-thermal centrifuged, washed, after drying, 700 DEG C under argon hydrogen mixed atmosphere
Lower calcining 3 hours, then obtains metal@mesoporous carbon spheres (Pd-Cu@mCS).
Fig. 2 is that the TEM of catalyst made from the present embodiment schemes, and the dash area in figure is the ground gold of embedded mesoporous carbon spheres
Metal particles.
Embodiment 3
A kind of metal nanoparticle is uniformly embedded into the controllable method for preparing of the elctro-catalyst of mesoporous carbon spheres internal structure：
(1) phenol: formaldehyde: melamine=4: the mixed liquor of 13: 1 mol ratios is configured；
(2) after reaction mixture is reacting 30 minutes for 65 DEG C in (1), the mass fraction for adding F127 is 4%；
(3) when in (2) mixed solution system continue to react 2 hours at 65 DEG C, the rear deionized water for adding 50mL, make its anti-
Answer 16 hours；
(4) reaction solution in (3) is mixed with deionized water volume with 2: 1, add palladium, copper precursor powder be respectively 1mg,
3mg, after pH of mixed is adjusted to 9.5；
(5) hydro-thermal 24 hours at 130 DEG C are respectively put into water heating kettle after mixed liquor in (4) is stirred；
(6) the obtained product after (5) hydro-thermal centrifuged, washed, after drying, 700 DEG C under argon hydrogen mixed atmosphere
Lower calcining 3 hours, then obtains metal@mesoporous carbon spheres (Pd-Cu@mCS).
Fig. 3 is that the TEM of catalyst made from the present embodiment schemes, and the dash area in figure is the ground gold of embedded mesoporous carbon spheres
Metal particles.
The structural parameters that elctro-catalyst Pd-Cu@mCS balls are made in embodiment 1-3 are as shown in table 1.
Table 1
| Embodiment | Aperture (nm) | Pore volume (cm3/g) | Specific surface area (m2/g) |
| Embodiment 1 | 3.2 | 0.35 | 542 |
| Embodiment 2 | 4.4 | 0.39 | 558 |
| Embodiment 3 | 1.9 | 0.47 | 571 |
Elctro-catalyst prepared by embodiment 1-3 carries out laboratory electro-catalysis denitrification test, and electrolyte is containing 500mg/L
The sodium nitrate of nitrogen and 0.1mol/L sodium sulphate mixed solution, denitrification effect is determined using electrochemical workstation, by elctro-catalyst
Working electrode is made, platinum plate electrode is used as to electrode, and standard calomel electrode is reference electrode.Respectively using ultraviolet spectrometry, N-
The concentration of nitrate, nitrite and ammonia nitrogen in (1- naphthyls)-ethylenediamine photometry and Na's reagent measure electrolyte.It is above-mentioned
The result of the test of 12 hours nitric efficiencies of elctro-catalyst and reaction selectivity is as shown in table 2.
Table 2
From table 2, Pd-Cu@mCS made from embodiment 1-3 have higher nitrate removal rate and good nitrogen
Selectivity, wherein, embodiment 3 has highest nitrate removal rate and optimal nitrogen in the Pd-Cu@mCS prepared by 700 DEG C
Selectivity.
Claims (10)
1. a kind of metal nanoparticle is uniformly embedded into the controllable method for preparing of the elctro-catalyst of mesoporous carbon spheres internal structure, its feature
It is, comprises the following steps that：
Step 1)：Phenol, formaldehyde, the mixed liquor of melamine are configured in proportion, are reacted；
Step 2)：F127 is added in reaction mixture made from step 1) to continue to react；
Step 3)：In mixed solution system made from step 2), water is added, makes its reaction overnight；
Step 4)：Reaction solution made from step 3) is mixed with deionized water, then adds metal precursor powder, then adjust mixed
Close the pH value of liquid；
Step 5)：Hydro-thermal in water heating kettle is put into after mixed liquor made from step 4) is stirred；
Step 6)：Product after the hydro-thermal that step 5) is obtained centrifuged, washed, being dried successively, calcine after, uniformly born
It is loaded with the noble metal@mesoporous carbon spheres of different-grain diameter size, i.e. Pd-Cu@mCS.
2. metal nanoparticle as claimed in claim 1 is uniformly embedded into the controllable of the elctro-catalyst of mesoporous carbon spheres internal structure
Preparation Method, it is characterised in that the mol ratio of phenol and formaldehyde is 5: 1~1: 5 in the step 1)；Formaldehyde and melamine rub
You are than being 100: 0~1: 20；Reaction condition is：At 40~100 DEG C, 10~300min is reacted.
3. metal nanoparticle as claimed in claim 1 is uniformly embedded into the controllable of the elctro-catalyst of mesoporous carbon spheres internal structure
Preparation Method, it is characterised in that F127 addition is the 0.1~30% of reaction mixture quality in the step 2)；Reaction
2~3h of time.
4. metal nanoparticle as claimed in claim 1 is uniformly embedded into the controllable of the elctro-catalyst of mesoporous carbon spheres internal structure
Preparation Method, it is characterised in that the addition of the step 3) reclaimed water is the 0.1~30% of reaction mixture volume；During reaction
Between be 6~30h.
5. metal nanoparticle as claimed in claim 1 is uniformly embedded into the controllable of the elctro-catalyst of mesoporous carbon spheres internal structure
Preparation Method, it is characterised in that in the step 4) volume ratio of reaction solution and deionized water be 1: 1~~1: 200；Metal front
Body powder palladium using gold and its compound, platinum and its compound, ruthenium and its compound, copper and its compound, Cobalt and compounds of cobalt,
Any one or a few composition in iron and its compound and sodium and its compound；PH value is adjusted to 8~12.
6. metal nanoparticle as claimed in claim 5 is uniformly embedded into the controllable of the elctro-catalyst of mesoporous carbon spheres internal structure
Preparation Method, it is characterised in that the metal precursor powder is using palladium sodium chlorate and the mixture of nitrate trihydrate copper, palladium sodium chlorate
Mol ratio with nitrate trihydrate copper is 1: 4~4: 1.
7. metal nanoparticle as claimed in claim 1 is uniformly embedded into the controllable of the elctro-catalyst of mesoporous carbon spheres internal structure
Preparation Method, it is characterised in that the temperature of hydro-thermal is 80~180 DEG C in the step 5), and the hydro-thermal time is 2-24h.
8. metal nanoparticle as claimed in claim 1 is uniformly embedded into the controllable of the elctro-catalyst of mesoporous carbon spheres internal structure
Preparation Method, it is characterised in that the atmosphere of calcining is argon hydrogen gaseous mixture in the step 6), and calcining heat is 300~900 DEG C, is forged
The burning time is 2~8h.
9. metal nanoparticle as claimed in claim 1 is uniformly embedded into the controllable of the elctro-catalyst of mesoporous carbon spheres internal structure
Preparation Method, it is characterised in that the Pd-Cu in the Pd-Cu@mCS that the step 6) obtains exists in the form of alloy.
10. metal nanoparticle as claimed in claim 1 is uniformly embedded into the controllable of the elctro-catalyst of mesoporous carbon spheres internal structure
Preparation method, it is characterised in that the pore-size distribution for the Pd-Cu@mCS that the step 6) obtains is 1.9~4.4nm, specific surface area
For 540~570m2/ g, pore volume scope are 0.3~0.5cm3/g。
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| CN108531932A (en) * | 2018-04-11 | 2018-09-14 | 郑州大学 | A kind of hollow carbon sphere encapsulation Ru nano particle electrolysis water catalyst and preparation method thereof |
| CN110465319A (en) * | 2019-08-23 | 2019-11-19 | 江西夏氏春秋环境股份有限公司 | A kind of preparation method and application of the copper palladium bimetal nano catalysis material of N doping |
| CN111111694A (en) * | 2020-01-20 | 2020-05-08 | 东华大学 | Preparation of copper-palladium bimetallic supported mesoporous carbon and carbon nanotube composite material |
| CN112592451A (en) * | 2020-12-15 | 2021-04-02 | 大连理工大学 | Polymer composite material with rough surface, nano carbon material, preparation method and application |
| WO2021078128A1 (en) * | 2019-10-22 | 2021-04-29 | 中国科学院青岛生物能源与过程研究所 | Method for preparing mesoporous carbon supported metal nanoparticle catalyst |
| CN114917930A (en) * | 2022-05-18 | 2022-08-19 | 东华大学 | Copper-palladium metal loaded mesoporous carbon-coated carbon nanotube one-dimensional nanofiber material and preparation method thereof |
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| CN108531932A (en) * | 2018-04-11 | 2018-09-14 | 郑州大学 | A kind of hollow carbon sphere encapsulation Ru nano particle electrolysis water catalyst and preparation method thereof |
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| WO2021078128A1 (en) * | 2019-10-22 | 2021-04-29 | 中国科学院青岛生物能源与过程研究所 | Method for preparing mesoporous carbon supported metal nanoparticle catalyst |
| CN111111694A (en) * | 2020-01-20 | 2020-05-08 | 东华大学 | Preparation of copper-palladium bimetallic supported mesoporous carbon and carbon nanotube composite material |
| CN111111694B (en) * | 2020-01-20 | 2021-03-19 | 东华大学 | Preparation of copper-palladium bimetallic supported mesoporous carbon and carbon nanotube composite material |
| CN112592451A (en) * | 2020-12-15 | 2021-04-02 | 大连理工大学 | Polymer composite material with rough surface, nano carbon material, preparation method and application |
| CN114917930A (en) * | 2022-05-18 | 2022-08-19 | 东华大学 | Copper-palladium metal loaded mesoporous carbon-coated carbon nanotube one-dimensional nanofiber material and preparation method thereof |
| CN114917930B (en) * | 2022-05-18 | 2024-01-26 | 东华大学 | Copper-palladium metal loaded mesoporous carbon coated carbon nanotube one-dimensional nanofiber material and preparation method thereof |
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Application publication date: 20180119 |