CN108772089A - A kind of N doping, carbon with netural net structure connect the preparation method of phosphating sludge high-performance liberation of hydrogen catalyst - Google Patents
A kind of N doping, carbon with netural net structure connect the preparation method of phosphating sludge high-performance liberation of hydrogen catalyst Download PDFInfo
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- CN108772089A CN108772089A CN201810515256.4A CN201810515256A CN108772089A CN 108772089 A CN108772089 A CN 108772089A CN 201810515256 A CN201810515256 A CN 201810515256A CN 108772089 A CN108772089 A CN 108772089A
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- doping
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- 239000010802 sludge Substances 0.000 title claims abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000001257 hydrogen Substances 0.000 title claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 title claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 16
- 239000004640 Melamine resin Substances 0.000 claims abstract description 16
- 239000006260 foam Substances 0.000 claims abstract description 16
- 206010001497 Agitation Diseases 0.000 claims abstract description 10
- 238000013019 agitation Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010521 absorption reaction Methods 0.000 claims abstract description 5
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 5
- 239000004202 carbamide Substances 0.000 claims abstract description 5
- 235000019837 monoammonium phosphate Nutrition 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 4
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 abstract description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 abstract description 2
- 229940010552 ammonium molybdate Drugs 0.000 abstract description 2
- 239000011609 ammonium molybdate Substances 0.000 abstract description 2
- 235000013877 carbamide Nutrition 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 abstract description 2
- 229910021641 deionized water Inorganic materials 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The present invention provides the preparation method of a kind of N doping with netural net structure, carbon connection phosphating sludge high-performance liberation of hydrogen catalyst, includes the following steps：It weighs a certain amount of ammonium molybdate, ammonium dihydrogen phosphate and urea to be dissolved in deionized water, magnetic agitation is allowed to be completely dissolved, this solution is placed in oil bath, is aged under the conditions of 80 DEG C of magnetic agitations.Then, it takes the melamine resin foam of one piece of clean dried to be put into above-mentioned solution, continues to stir certain time.Then, the melamine resin foam of taking-up absorption above-mentioned solution completely, which is placed in baking oven, dries, obtain phosphating sludge precursor species, and presoma is put into tube furnace and is calcined under nitrogen atmosphere, it finally naturally cools to room temperature and connects phosphating sludge high-performance liberation of hydrogen catalyst to get to a kind of N doping, carbon with netural net structure.The method of the present invention it is of low cost, production technology is easily-controllable, and morphology and size uniformity is preferable, and have higher Hydrogen Evolution Performance, be suitble to large-scale industrial production.
Description
Technical field
The present invention a kind of N doping, carbon with netural net structure connect the system of phosphating sludge high-performance liberation of hydrogen catalyst
Preparation Method, it is characterized in that preparing netural net by calcination method using melamine resin foam as template more particularly to one kind
The N doping of structure, the preparation method of carbon connection phosphating sludge high-performance liberation of hydrogen catalyst.
Background technology
In recent years, phosphating sludge is due to good metallic conductivity, being that good H transmits substance, having class rhodium, palladium
The property of noble metal, and good stability is all had in acid-alkali medium, it is considered to be a kind of liberation of hydrogen with fine foreground
Elctro-catalyst.It finds, is but rarely reported about probing into its appearance structure is studied, therefore design and prepare with not through consulting
Phosphating sludge with appearance structure has important significant and material science forward position a research field to become more and more important.
Template is to prepare a kind of simply and effectively method of special appearance structural material, pattern that can be to material, size
Etc. being regulated and controled.Melamine resin foam is cheap and easy to get, has 3D reticular structures, is used as template to prepare some materials
Material.
The present invention is avoided using melamine resin foam as template, while as carbon source and nitrogen source due to high temperature sintering
Caused by nanoparticle agglomerates, and the later stage is without going removing template, preparation process simple.
Invention content
The present invention relates to a kind of, and N doping, carbon with netural net structure connect phosphating sludge high-performance liberation of hydrogen catalyst
Preparation method, and in particular to using melamine resin foam as template by calcination method synthesized have netural net structure
N doping, carbon connect phosphating sludge high-performance liberation of hydrogen catalyst, preparation process is simple, is easy to produce in batches.
The present invention uses following technical scheme：
It weighs a certain amount of soluble ammonium molybdate, ammonium dihydrogen phosphate and urea to be dissolved in deionized water, magnetic agitation makes
Be completely dissolved to after forming clear transparent solutions, this solution is placed in oil bath, is aged under the conditions of 80 DEG C of magnetic agitations 5 small
When, then, the melamine resin foam (30mm × 10mm × 10mm) of one piece of clean dried is taken, is put into above-mentioned solution,
Continue stirring 5 hours under the conditions of 80 DEG C, so that it is fully removed air entrapment and adsorb above-mentioned solution completely.Then, absorption is taken out
The melamine resin foam of complete above-mentioned solution is placed in 80 DEG C of baking oven, is dried 12 hours, is obtained phosphating sludge presoma object
Matter finally puts this presoma in tube furnace into, in a nitrogen atmosphere, certain temperature is heated to certain heating rate, protects
Warm certain time, then naturally cool to room temperature, you can obtain a kind of N doping, carbon connection phosphorus with netural net structure
Change molybdenum high-performance liberation of hydrogen catalyst.
Product Process involved in the present invention simply easily realizes that product quality is stable and process repeatability can be good, it is easy to accomplish
Prepared by mass, raw material are cheap and easy to get, response parameter is easy to control, securely and reliably, it is economical convenient and be easy to amplification and work
The advantages that industry metaplasia is produced, the liberation of hydrogen catalyst morphology and dimensional homogeneity of gained are preferable.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) pattern photo of product shown in embodiment 1；
Specific implementation mode
Embodiment 1
It weighs 0.2mmol ammonium molybdates, 1.4mmol ammonium dihydrogen phosphates and 0.033mmol urea and is dissolved in 80mL deionized waters
In, magnetic agitation is allowed to be completely dissolved to form clear transparent solutions, this solution is placed in oil bath, in 80 DEG C of magnetic agitation conditions
Lower ageing 5 hours.The melamine resin foam (30mm × 10mm × 10mm) of one piece of clean dried is added, and in 80 DEG C of conditions
Under continue stirring 5 hours, so that it is fully removed air entrapment and adsorb above-mentioned solution completely；Then, it is completely above-mentioned to take out absorption
The melamine resin foam of solution is placed in 80 DEG C of baking oven, is dried 12 hours, is obtained phosphating sludge precursor species, finally will
This presoma is put into tube furnace, and in a nitrogen atmosphere, 900 DEG C of soaking time is then naturally cooled in 2h in tube furnace
Room temperature, you can obtain a kind of N doping, carbon connection phosphating sludge high-performance liberation of hydrogen catalyst with netural net structure, mistake
Current potential is 125mV, Tafel slope 53mV/dec.
Embodiment 2
It weighs 0.2mmol ammonium molybdates, 1.4mmol ammonium dihydrogen phosphates and 0.033mmol urea and is dissolved in 80mL deionized waters
In, magnetic agitation is allowed to be completely dissolved to form clear transparent solutions, this solution is placed in oil bath, in 80 DEG C of magnetic agitation conditions
Lower ageing 5 hours.The melamine resin foam (30mm × 10mm × 10mm) of one piece of clean dried is added, and in 80 DEG C of conditions
Under continue stirring 5 hours, so that it is fully removed air entrapment and adsorb above-mentioned solution completely；Then, it is completely above-mentioned to take out absorption
The melamine resin foam of solution is placed in 80 DEG C of baking oven, is dried 12 hours, is obtained phosphating sludge precursor species, finally will
This presoma is put into tube furnace, and in a nitrogen atmosphere, 850 DEG C of soaking time is then naturally cooled in 3h in tube furnace
Room temperature, you can obtain a kind of N doping, carbon connection phosphating sludge high-performance liberation of hydrogen catalyst with netural net structure, mistake
Current potential is 125mV, Tafel slope 53mV/dec.
It should be understood that for those of ordinary skills, it can be modified or changed according to the above description,
And these improvement of institute or transformation should all belong to the protection domain of appended claims of the present invention.
Claims (6)
1. a kind of N doping, carbon with netural net structure connect the preparation method of phosphating sludge high-performance liberation of hydrogen catalyst,
It is characterized in that preparing the nitrogen of netural net structure by calcination method using melamine resin foam as template more particularly to one kind
Doping, carbon connect the preparation method of phosphating sludge high-performance liberation of hydrogen catalyst, and specific preparation process is：Weigh 0.2mmol ammonium molybdates,
1.4mmol ammonium dihydrogen phosphates and 0.033mmol urea are dissolved in 80mL deionized waters, and magnetic agitation is allowed to be completely dissolved to be formed
This solution is placed in oil bath by clear transparent solutions, is aged 5 hours under the conditions of 80 DEG C of magnetic agitations；It is dry that one piece of cleaning is added
Dry melamine resin foam (30mm × 10mm × 10mm), and continue stirring 5 hours under the conditions of 80 DEG C, so that it is fully gone
Above-mentioned solution is adsorbed except air entrapment and completely；Then, the melamine resin foam for taking out absorption above-mentioned solution completely is placed in
In 80 DEG C of baking oven, dries 12 hours, obtain phosphating sludge precursor species, finally put this presoma in tube furnace into, in nitrogen
Under gas atmosphere, certain temperature is heated to certain heating rate, held for some time then naturally cools to room temperature, you can
Obtain a kind of N doping, carbon connection phosphating sludge high-performance liberation of hydrogen catalyst with netural net structure.
2. according to the method described in claim 1, it is characterized in that：Using melamine resin foam as template, while as carbon
Source has synthesized N doping, carbon with netural net structure with nitrogen source and has connected phosphating sludge high-performance liberation of hydrogen catalyst, avoids
Due to nanoparticle agglomerates caused by high temperature sintering, solve the problems, such as that the control of phosphating sludge liberation of hydrogen catalyst morphology is difficult, and the later stage
Without removing removing template.
3. preparation method according to claim 1, it is characterised in that heating rate when preparing presoma in tube furnace
Control is between 2-5 DEG C/min.
4. preparation method according to claim 1, it is characterised in that between the holding temperature is 850-900 DEG C.
5. preparation method according to claim 1, it is characterised in that soaking time of the presoma in tube furnace is in 2h-3h
Between.
6. preparation method according to claim 1 obtained N doping, carbon connection phosphating sludge with netural net structure
High-performance liberation of hydrogen catalyst, overpotential 125mV, Tafel slope 53mV/dec.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810515256.4A CN108772089B (en) | 2018-05-25 | 2018-05-25 | Preparation method of nitrogen-doped carbon-connected molybdenum phosphide high-performance hydrogen evolution catalyst with neural network structure |
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| CN201810515256.4A CN108772089B (en) | 2018-05-25 | 2018-05-25 | Preparation method of nitrogen-doped carbon-connected molybdenum phosphide high-performance hydrogen evolution catalyst with neural network structure |
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| CN108772089A true CN108772089A (en) | 2018-11-09 |
| CN108772089B CN108772089B (en) | 2021-06-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013617A (en) * | 2019-12-28 | 2020-04-17 | 山东大学 | One-dimensional molybdenum phosphide nanorod and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107362818A (en) * | 2017-07-12 | 2017-11-21 | 武汉理工大学 | Nitrogen phosphorus codope carbon coating transition metal diphosphide liberation of hydrogen catalyst and preparation method |
| CN107999105A (en) * | 2018-01-06 | 2018-05-08 | 青岛科技大学 | A kind of preparation method of the phosphating sludge liberation of hydrogen catalyst with bar-shaped porous appearance structure |
| CN111013617A (en) * | 2019-12-28 | 2020-04-17 | 山东大学 | One-dimensional molybdenum phosphide nanorod and preparation method and application thereof |
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- 2018-05-25 CN CN201810515256.4A patent/CN108772089B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107362818A (en) * | 2017-07-12 | 2017-11-21 | 武汉理工大学 | Nitrogen phosphorus codope carbon coating transition metal diphosphide liberation of hydrogen catalyst and preparation method |
| CN107999105A (en) * | 2018-01-06 | 2018-05-08 | 青岛科技大学 | A kind of preparation method of the phosphating sludge liberation of hydrogen catalyst with bar-shaped porous appearance structure |
| CN111013617A (en) * | 2019-12-28 | 2020-04-17 | 山东大学 | One-dimensional molybdenum phosphide nanorod and preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013617A (en) * | 2019-12-28 | 2020-04-17 | 山东大学 | One-dimensional molybdenum phosphide nanorod and preparation method and application thereof |
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