CN109759044A - A kind of method of prepare with scale for the cathod catalyst of electrochemistry formated ammonia - Google Patents
A kind of method of prepare with scale for the cathod catalyst of electrochemistry formated ammonia Download PDFInfo
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Abstract
A kind of method the invention discloses prepare with scale for the cathod catalyst of electrochemistry formated ammonia, belongs to electrochemistry formated ammonia catalyst technical field.Technical solution of the present invention main points are as follows: a kind of method of prepare with scale for the cathod catalyst of electrochemistry formated ammonia, is prepared on carbon paper by carbon-based stratified nano materials and adhesive coated.The present invention provides electrochemistry formated ammonia cathod catalysts that is a kind of environmental-friendly, easy to operate, low in cost and being produced on a large scale; the material is with its good electric conductivity, material surface fold-like structures abundant and high nitrogen content; excellent electrochemical catalysis nitrogen activity is shown at normal temperatures and pressures, makes it that there is certain practical value in the industrial applications field of electrochemistry formated ammonia.
Description
Technical field
The invention belongs to electrochemistry formated ammonia catalyst technical fields, and in particular to a kind of prepare with scale is used for electrochemistry
The method for synthesizing the cathod catalyst of ammonia.
Background technique
Ammonia is the important component of chemical fertilizer, it plays a crucial role the survival and development of the mankind.Currently, industrial
Upper synthesis ammonia mainly uses aber process, carries out at high temperature and pressure (150-350atm, 350-550 DEG C), the synthesis of this harshness
Condition consumes the energy supply of the whole world about 1%-2% every year.In addition, traditional aber process synthesis ammonia needs hydrogen as former
One of material, and the process of traditional hydrogen manufacturing can discharge a large amount of CO2.These above-mentioned unfavorable factors undoubtedly increase energy burden, simultaneously
Bring new problem of environmental pollution.Therefore, the catalysis reaction for exploring synthesis ammonia in a mild condition is just particularly important.Nitrogen
Pneumoelectric electronation ammonia synthesis reaction can carry out at normal temperatures and pressures, and can source by water as hydrogen, so as to cause
The extensive concerns of researchers.Efficient elctro-catalyst plays a crucial role electrochemistry formated ammonia, mesh
Preceding electrochemistry formated ammonia catalyst mainly has noble metal catalyst and non-precious metal catalyst, and wherein noble metal catalyst is mainly
The catalyst of the elements such as platiniferous, ruthenium, palladium and gold, such as El-Sayed M. A.(Nano Energy 2018,49,316-
323) by preparing the catalysis material of gold nanometer cage structure, realizing that electrochemistry produces ammonia rate is 3.9 μ g h−1 cm−2；Yan Junmin
Deng (Adv. Mater. 2017,29,1606550) by modifying gold in TiO2On, so that preparation produces ammonia rate and is
21.4μg h−1 mg−1 cat.Catalyst；Once outstanding equal (Adv. Mater. 2018,30,1803498) was by by monatomic ruthenium
Modification produces ammonia rate (120.9 μ g h in nitrogenous carbon material surface, to greatly improve−1 mg−1 cat.).Noble metal catalyst
With the advantage in performance, but easily poisoning, service life is short and expensive, it is made to be difficult to meet the needs in actual production.
Common non-precious metal catalyst is mainly transition metal carbon/nitrogen/oxygen/sulfide catalyst, such as Sun Xu equality passes through synthesis
Mo2N nanometer rods (Chem. Commun., 2018,54,8474-8477) and MoS2Nano flower (Adv. Energy Mater.
2018,1801357) catalyst of structure, realizing produce ammonia rate respectively is 78.4 μ g h−1 mg−1 cat.With 29.28 μ g h−1
mg−1 cat..Although non-precious metal catalyst has the advantage in price, but its synthesis step is often relatively complicated and produces in the process
Raw waste liquid is also difficult to meet the actual demand in industry due to needing to be further processed containing heavy metal ion.Therefore
And the non-metallic catalyst for capableing of high-efficiency electrochemical reduction nitrogen synthesis ammonia is developed, really realize the work of electrochemistry formated ammonia
Industry application has certain practical value.Based on this, researchers, which design, has synthesized a variety of non-metal base catalyst,
Such as it is complete it is mediate (ACS Catal. 2018,8,1,186 1191) by ZIF-8 as presoma, the carbon-based catalysis material that synthesizes
It is 27.2 μ g h that material, which realizes and produces ammonia rate,−1 mg−1 cat.；Sun Xu equality (Nat. Commun. 2018,9,3485) is to be carbonized
Boron is catalyst, and realizing and producing ammonia rate is 26.57 μ g h−1 mg−1 cat..However, existing non-metal base catalyst is equal at present
It cannot achieve large-scale production, this greatly hinders the process of industrialization of electrochemistry formated ammonia.
Summary of the invention
Present invention solves the technical problem that be overcome in existing electrochemistry formated ammonia technology noble metal catalyst it is expensive,
Non-precious metal catalyst preparation process is complicated and non-metal base catalyst can not large-scale production defect, and provide one
Method of the kind prepare with scale for the cathod catalyst of electrochemistry formated ammonia.
The present invention adopts the following technical scheme that a kind of prepare with scale is used for electrochemistry formated to solve above-mentioned technical problem
The method of the cathod catalyst of ammonia, it is characterised in that detailed process are as follows:
Step S1: obtaining material A after melamine presoma is sufficiently crushed, wherein melamine presoma is melamine sea
Continuous, melamine foamed plastic or melamine powder, are transferred to magnetic boat for material A and are placed in tube furnace, in atmosphere of inert gases
Middle elder generation is warming up to 300 DEG C through 1h by room temperature and keeps 2h, then is warming up to 550 DEG C with the heating rate of 5 DEG C/min and keeps 2h, so
Cooled to room temperature obtains material B afterwards；
Step S2: material B is placed in high purity water and is impregnated to remove inorganic salt impurities ion remaining in material, then uses high purity water
Progress filtering and washing, which is placed in air dry oven, obtains carbon-based stratified nano materials in 40-60 DEG C of dry 12h, the carbon-based stratiform
The lattice fringe of nano material is 0.34nm, and meeting Graphitic carbon structure has good electric conductivity, while carbon-based laminar nano material
Expect that surface is distributed in accordion, for promoting the contact area of nitrogen and electrolyte and catalyst；
Step S3: being made ink for being uniformly mixed after carbon-based stratified nano materials addition binder solution with dehydrated alcohol and water,
Ink is evenly applied on carbon paper again, then coated carbon paper is made to the yin for being used for electrochemistry formated ammonia in drying at room temperature
Electrode catalyst.
Preferably, melamine presoma described in step S1 carries out abundant powder using pulverizer or glass mortar grinding
It is broken.
Preferably, inert gas described in step S1 is nitrogen or argon gas.
Preferably, the charge ratio of carbon-based stratified nano materials and binder solution described in step S3 is 5-15mg:30-
50μL。
Preferably, binder described in step S3 is polytetrafluoroethylene (PTFE), Kynoar, polyvinyl alcohol, carboxymethyl cellulose
One of plain sodium or Nafion.
Preferably, carbon paper described in step S3 is hydrophobicity carbon paper or hydrophilic carbon paper.
Method of the prepare with scale of the present invention for the cathod catalyst of electrochemistry formated ammonia, it is characterised in that tool
Body step are as follows:
Step S1: material A is obtained after 3g melamine sponge is sufficiently crushed using pulverizer, material A is transferred to magnetic boat simultaneously
It is placed in tube furnace, is first warming up to 300 DEG C through 1h by room temperature in nitrogen atmosphere and keeps 2h, then with the heating speed of 5 DEG C/min
Rate is warming up to 550 DEG C and keeps 2h, and then cooled to room temperature obtains material B；
Step S2: material B is placed in high purity water and is impregnated to remove inorganic salt impurities ion remaining in material, then uses high purity water
Progress filtering and washing, which is placed in air dry oven, obtains carbon-based stratified nano materials in 50 DEG C of dry 12h, which receives
The lattice fringe of rice material is 0.34nm, and meeting Graphitic carbon structure has good electric conductivity, while carbon-based stratified nano materials
Surface is distributed in accordion, for promoting the contact area of nitrogen and electrolyte and catalyst；
Step S3: by the nothing for being 3:1 with volume ratio after 10mg 40 μ L Nafion binder solutions of carbon-based stratified nano materials addition
Water-ethanol and water, which are uniformly mixed, is made ink, then 10 μ L inks are evenly applied to 1*1cm2Carbon paper on, then will coat
Carbon paper the cathod catalyst for electrochemistry formated ammonia is made in drying at room temperature；
Electrochemistry formated ammonia is carried out on electrochemistry formated ammonia reaction unit, using silver/silver chloride electrode as reference electrode, stone
Inker is used as to electrode, and cathode use the cathod catalyst of above-mentioned preparation as working electrode, used between anode and cathode Nafion membrane every
It opens, with 0.1mol L−1Hydrochloric acid solution be electrolyte, cathode chamber is continually fed into nitrogen or air in synthesis process, normal in room temperature
Pressure carries out electrochemistry formated ammonia, and the yield that ammonia is obtained after the operating at voltages 2h of -0.7V is 19.52 μ g h−1 mg−1 cat.。
Compared with the prior art, the invention has the following beneficial effects:
1, the present invention in using it is cheap and can mass production different existence forms melamine as presoma, by one
Step carbonisation directly prepares the catalysis material of electrochemistry formated ammonia, the lattice item of prepared carbon-based stratified nano materials
Line is 0.34nm, meets Graphitic carbon structure, it was demonstrated that the catalysis material has good electric conductivity.Meanwhile it being prepared carbon-based
Stratified nano materials surface is distributed in accordion, improves the contact area of nitrogen and electrolyte and catalyst.In addition, high contains
Nitrogen quantity significant increase catalytic active site points, ensure that nitrogen in catalytic process with effective combination of catalyst.
2, the carbon-based stratified nano materials obtained by the present invention realize the purpose of electrochemistry formated ammonia under normal temperature and pressure, pole
The earth reduces energy consumption.
3, the present invention can directly use air as nitrogen gas source electrochemistry formated ammonia, be greatly enriched raw material sources,
Reduce the preparation cost of synthesis ammonia.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of carbon-based stratified nano materials made from the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope picture of carbon-based stratified nano materials made from the embodiment of the present invention 1；
Fig. 3 is the x-ray photoelectron spectroscopy figure of carbon-based stratified nano materials made from the embodiment of the present invention 1；
Fig. 4 is the generating rate figure of the electrochemistry formated ammonia of cathod catalyst made from 1-3 of the embodiment of the present invention；
Fig. 5 is the structural schematic diagram of electrochemistry formated ammonia reaction unit.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
Step S1: material A 1 is obtained after 3g melamine sponge is sufficiently crushed using pulverizer, material A 1 is transferred to magnetic boat
It is placed in tube furnace, is first warming up to 300 DEG C through 1h by room temperature in nitrogen atmosphere and keeps 2h, then with the heating of 5 DEG C/min
Rate is warming up to 550 DEG C and keeps 2h, and then cooled to room temperature obtains material B1；
Step S2: material B1 being placed in high purity water and is impregnated to remove inorganic salt impurities ion remaining in material, then with high-purity
Water progress filtering and washing, which is placed in air dry oven, obtains carbon-based stratified nano materials in 50 DEG C of dry 12h, the carbon-based stratiform
The lattice fringe of nano material is 0.34nm, and meeting Graphitic carbon structure has good electric conductivity, while carbon-based laminar nano material
Expect that surface is distributed in accordion, for promoting the contact area of nitrogen and electrolyte and catalyst；
Step S3: by the nothing for being 3:1 with volume ratio after 10mg 40 μ L Nafion binder solutions of carbon-based stratified nano materials addition
Water-ethanol and water, which are uniformly mixed, is made ink, then 10 μ L inks are evenly applied to 1*1cm2Carbon paper on, then will coat
Carbon paper the cathod catalyst for electrochemistry formated ammonia is made in drying at room temperature；
Electrochemistry formated ammonia is carried out on electrochemistry formated ammonia reaction unit, using silver/silver chloride electrode as reference electrode, stone
Inker is used as to electrode, and cathode use the cathod catalyst of above-mentioned preparation as working electrode, used between anode and cathode Nafion membrane every
It opens, with 0.1mol L−1Hydrochloric acid solution be electrolyte, cathode chamber is continually fed into nitrogen or air in synthesis process, normal in room temperature
Pressure carries out electrochemistry formated ammonia, in -0.7V(vsRHE the yield that ammonia is obtained after operating at voltages 2h) is 19.52 μ g h−1
mg−1 cat.(as shown in Figure 4).
Embodiment 2
Step S1: material A 2 is obtained after 3g melamine foamed plastic is sufficiently crushed using pulverizer, material A 2 is transferred to magnetic boat
It is placed in tube furnace, is first warming up to 300 DEG C through 1h by room temperature in nitrogen atmosphere and keeps 2h, then with the heating of 5 DEG C/min
Rate is warming up to 550 DEG C and keeps 2h, and then cooled to room temperature obtains material B2；
Step S2: material B2 being placed in high purity water and is impregnated to remove inorganic salt impurities ion remaining in material, then with high-purity
Water progress filtering and washing, which is placed in air dry oven, obtains carbon-based stratified nano materials in 40 DEG C of dry 12h, the carbon-based stratiform
The lattice fringe of nano material is 0.34nm, and meeting Graphitic carbon structure has good electric conductivity, while carbon-based laminar nano material
Expect that surface is distributed in accordion, for promoting the contact area of nitrogen and electrolyte and catalyst；
Step S3: by the nothing for being 3:1 with volume ratio after 10mg 40 μ L Nafion binder solutions of carbon-based stratified nano materials addition
Water-ethanol and water, which are uniformly mixed, is made ink, then 10 μ L inks are evenly applied to 1*1cm2Carbon paper on, then will coat
Carbon paper the cathod catalyst for electrochemistry formated ammonia is made in drying at room temperature；
Electrochemistry formated ammonia is carried out on electrochemistry formated ammonia reaction unit, using silver/silver chloride electrode as reference electrode, stone
Inker is used as to electrode, and cathode use the cathod catalyst of above-mentioned preparation as working electrode, used between anode and cathode Nafion membrane every
It opens, with 0.1mol L−1Hydrochloric acid solution be electrolyte, cathode chamber is continually fed into nitrogen or air in synthesis process, normal in room temperature
Pressure carries out electrochemistry formated ammonia, in -0.7V(vsRHE the yield that ammonia is obtained after operating at voltages 2h) is 15.43 μ g h−1
mg−1 cat.(as shown in Figure 4).
Embodiment 3
Step S1: obtaining material A 3 after 3g melamine powder is fully ground in glass mortar, material A 3 is transferred to magnetic
Boat is placed in tube furnace, is first warming up to 300 DEG C through 1h by room temperature in nitrogen atmosphere and is kept 2h, then with the liter of 5 DEG C/min
Warm rate is warming up to 550 DEG C and keeps 2h, and then cooled to room temperature obtains material B3；
Step S2: material B3 being placed in high purity water and is impregnated to remove inorganic salt impurities ion remaining in material, then with high-purity
Water progress filtering and washing, which is placed in air dry oven, obtains carbon-based stratified nano materials in 60 DEG C of dry 12h, the carbon-based stratiform
The lattice fringe of nano material is 0.34nm, and meeting Graphitic carbon structure has good electric conductivity, while carbon-based laminar nano material
Expect that surface is distributed in accordion, for promoting the contact area of nitrogen and electrolyte and catalyst；
Step S3: by the nothing for being 3:1 with volume ratio after 10mg 40 μ L Nafion binder solutions of carbon-based stratified nano materials addition
Water-ethanol and water, which are uniformly mixed, is made ink, then 10 μ L inks are evenly applied to 1*1cm2Carbon paper on, then will coat
Carbon paper the cathod catalyst for electrochemistry formated ammonia is made in drying at room temperature；
Electrochemistry formated ammonia is carried out on electrochemistry formated ammonia reaction unit, using silver/silver chloride electrode as reference electrode, stone
Inker is used as to electrode, and cathode use the cathod catalyst of above-mentioned preparation as working electrode, used between anode and cathode Nafion membrane every
It opens, with 0.1mol L−1Hydrochloric acid solution be electrolyte, cathode chamber is continually fed into nitrogen or air in synthesis process, normal in room temperature
Pressure carries out electrochemistry formated ammonia, in -0.7V(vsRHE the yield that ammonia is obtained after operating at voltages 2h) is 13.34 μ g h−1
mg−1 cat.(as shown in Figure 4).
Synthesis ammonia experiment is carried out on electrochemistry formated ammonia reaction unit (as shown in Figure 5), is made using silver/silver chloride electrode
For reference electrode, graphite rod is used as to electrode, and cathode uses the above-mentioned cathod catalyst prepared as working electrode, anode and cathode it
Between separated with Nafion membrane, with 0.1mol L−1Hydrochloric acid solution be electrolyte.In experimentation cathode chamber be continually fed into nitrogen or
Air carries out the experiment of electrochemistry formated ammonia at normal temperatures and pressures.After the operating at voltages 2h of -0.7V, cathode chamber is drawn
Electrolyte 2mL sequentially adds 2mL colorant (L containing 1mol−1Sodium hydroxide, 5wt% salicylic acid, 5wt% sodium citrate), 1mL oxygen
Agent (0.05mol L−1Sodium hypochlorite) and 0.2mL catalyst (1wt% sodium nitroprusside), solution prepares uniformly mixed, keeps away
After light stands 2h, the ultraviolet-visible absorption spectroscopy of solution is measured, analysis obtains the ammonia content in solution, and the generating rate of ammonia is by such as
Lower formula calculates:
NH3Yield=(cNH3 × V) / (17 × t × m)
Wherein cNH3To measure obtained NH3Concentration, V are cathode chamber electrolyte volumes, and t is the reaction time, and m is practical on carbon paper
The catalyst quality of appendix.
The present invention is not limited to the above embodiments, and the above embodiments and description only describe of the invention
Principle, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are fallen
Enter in the scope of protection of the invention.
Claims (7)
1. a kind of method of prepare with scale for the cathod catalyst of electrochemistry formated ammonia, it is characterised in that detailed process are as follows:
Step S1: obtaining material A after melamine presoma is sufficiently crushed, wherein melamine presoma is melamine sea
Continuous, melamine foamed plastic or melamine powder, are transferred to magnetic boat for material A and are placed in tube furnace, in atmosphere of inert gases
Middle elder generation is warming up to 300 DEG C through 1h by room temperature and keeps 2h, then is warming up to 550 DEG C with the heating rate of 5 DEG C/min and keeps 2h, so
Cooled to room temperature obtains material B afterwards；
Step S2: material B is placed in high purity water and is impregnated to remove inorganic salt impurities ion remaining in material, then uses high purity water
Progress filtering and washing, which is placed in air dry oven, obtains carbon-based stratified nano materials in 40-60 DEG C of dry 12h, the carbon-based stratiform
The lattice fringe of nano material is 0.34nm, and meeting Graphitic carbon structure has good electric conductivity, while carbon-based laminar nano material
Expect that surface is distributed in accordion, for promoting the contact area of nitrogen and electrolyte and catalyst；
Step S3: being made ink for being uniformly mixed after carbon-based stratified nano materials addition binder solution with dehydrated alcohol and water,
Ink is evenly applied on carbon paper again, then coated carbon paper is made to the yin for being used for electrochemistry formated ammonia in drying at room temperature
Electrode catalyst.
2. method of the prepare with scale according to claim 1 for the cathod catalyst of electrochemistry formated ammonia, feature
Be: melamine presoma described in step S1 is sufficiently crushed using pulverizer or glass mortar grinding.
3. method of the prepare with scale according to claim 1 for the cathod catalyst of electrochemistry formated ammonia, feature
Be: inert gas described in step S1 is nitrogen or argon gas.
4. method of the prepare with scale according to claim 1 for the cathod catalyst of electrochemistry formated ammonia, feature
Be: the charge ratio of carbon-based stratified nano materials and binder solution described in step S3 is 5-15mg:30-50 μ L.
5. method of the prepare with scale according to claim 1 for the cathod catalyst of electrochemistry formated ammonia, feature
Be: binder described in step S3 be polytetrafluoroethylene (PTFE), Kynoar, polyvinyl alcohol, sodium carboxymethylcellulose or
One of Nafion.
6. method of the prepare with scale according to claim 1 for the cathod catalyst of electrochemistry formated ammonia, feature
Be: carbon paper described in step S3 is hydrophobicity carbon paper or hydrophilic carbon paper.
7. method of the prepare with scale according to claim 1 for the cathod catalyst of electrochemistry formated ammonia, feature
It is specific steps are as follows:
Step S1: material A is obtained after 3g melamine sponge is sufficiently crushed using pulverizer, material A is transferred to magnetic boat simultaneously
It is placed in tube furnace, is first warming up to 300 DEG C through 1h by room temperature in nitrogen atmosphere and keeps 2h, then with the heating speed of 5 DEG C/min
Rate is warming up to 550 DEG C and keeps 2h, and then cooled to room temperature obtains material B；
Step S2: material B is placed in high purity water and is impregnated to remove inorganic salt impurities ion remaining in material, then uses high purity water
Progress filtering and washing, which is placed in air dry oven, obtains carbon-based stratified nano materials in 50 DEG C of dry 12h, which receives
The lattice fringe of rice material is 0.34nm, and meeting Graphitic carbon structure has good electric conductivity, while carbon-based stratified nano materials
Surface is distributed in accordion, for promoting the contact area of nitrogen and electrolyte and catalyst；
Step S3: by the nothing for being 3:1 with volume ratio after 10mg 40 μ L Nafion binder solutions of carbon-based stratified nano materials addition
Water-ethanol and water, which are uniformly mixed, is made ink, then 10 μ L inks are evenly applied to 1*1cm2Carbon paper on, then will coat
Carbon paper the cathod catalyst for electrochemistry formated ammonia is made in drying at room temperature；
Electrochemistry formated ammonia is carried out on electrochemistry formated ammonia reaction unit, using silver/silver chloride electrode as reference electrode, stone
Inker is used as to electrode, and cathode use the cathod catalyst of above-mentioned preparation as working electrode, used between anode and cathode Nafion membrane every
It opens, with 0.1mol L−1Hydrochloric acid solution be electrolyte, cathode chamber is continually fed into nitrogen or air in synthesis process, normal in room temperature
Pressure carries out electrochemistry formated ammonia, and the yield that ammonia is obtained after the operating at voltages 2h of -0.7V is 19.52 μ g h−1 mg−1 cat.。
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| CN110639489A (en) * | 2019-08-30 | 2020-01-03 | 中国科学院广州能源研究所 | Application of municipal sludge biochar in electrochemical synthesis of ammonia |
| CN111058054A (en) * | 2020-01-03 | 2020-04-24 | 大连理工大学 | Device and method for synthesizing ammonia by electrocatalytic nitrogen reduction by using salt bridge to replace Nafion membrane |
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Application publication date: 20190517 |