CN106944119A - A kind of carbonitride loads the preparation method of monoatomic metal catalysis material - Google Patents
A kind of carbonitride loads the preparation method of monoatomic metal catalysis material Download PDFInfo
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- CN106944119A CN106944119A CN201710172875.3A CN201710172875A CN106944119A CN 106944119 A CN106944119 A CN 106944119A CN 201710172875 A CN201710172875 A CN 201710172875A CN 106944119 A CN106944119 A CN 106944119A
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
Abstract
The invention mainly relates to the preparation method that a kind of carbonitride loads monoatomic metal catalysis material, specifically a kind of preparation method of lamellar graphite phase carbon nitride load monoatomic metal M catalysis materials (M is the one or two or more kinds in Ag, Pd, Rh, Pt), belongs to catalysis material field.The present invention is by the way of metal precursor and the complexing of carbon nitrogen presoma, suppress the reunion of metallic atom by the interaction between metal center and part, one step pyrolytic carbon nitrogen presoma and metal precursor prepare carbonitride load monoatomic metal catalysis material, improve the stability and dispersiveness of monoatomic metal catalysis material.Metal is supported on the surface of lamellar graphite phase carbon nitride in the form of zero-valent state single atomic dispersion in material prepared by this method, and the species and component of carried metal atom can be regulated and controled as needed.
Description
Technical field
The invention mainly relates to the preparation method that a kind of carbonitride loads monoatomic metal catalysis material, specifically a kind of layer
The preparation of shape graphite phase carbon nitride load monoatomic metal M catalysis materials (M is the one or two or more kinds in Ag, Pd, Rh, Pt)
Method, belongs to catalysis material field.
Background technology：
It is monatomic catalysis for catalyst practical application it is significant (X.Yang, A.Wang, B.Qiao, J.Li,
J.Liu,T.Zhang.Accounts of Chemical Research,2013,46,1740-1748.).Global annual platinum production
The 50% of amount is all used for the three-way conversion device of automobile tail gas purification system.It is catalyzed in electrode catalyst of fuel cell, petrochemical industry
Selection hydrogenation is reformed, and the synthesis of various fine chemicals all largely relies on the precious metal catalysts such as efficient load type platinum, palladium
Agent.The elements such as Ag, Pd, Rh and Pt have important application in the catalytic conversion reaction of the multiple fields such as petrochemical industry, these
The research and development of the preparation method of the monatomic catalyst of element can substantially reduce catalyst cost, improve production efficiency.
Easily reunite in preparation and course of reaction when metal is monatomic, cause catalyst to inactivate.Therefore, metal list
The preparation of catalyst atom must be by a kind of carrier of excellent performance.g-C3N4It is a kind of polymeric material being only made up of C and N
Material, simple component, which is constituted, to be caused to g-C3N4Property regulation and control can be carried out by simple method, it is and total without significantly changing
Component.g-C3N4Polymer property make to g-C3N4Surface chemistry regulation and control can pass through molecular level modification and Surface Engineering
Carry out, while ensure that its structure has enough flexibilities, make g-C3N4Can as various inorganic nano-particles main body
Matrix, so as to prepare g-C3N4Based composites (W.Ong, L.Tan, Y.Ng, S.Yong, S.Chai.Chemical
Reviews,2016,116,7159-7329.)。
Therefore, we develop a kind of step pyrolytic carbon nitrogen presoma and metal precursor prepares carbonitride and loads monatomic gold
Belong to the new method of catalysis material.Metal is supported on lamellar graphite phase carbon nitride in the form of zero-valent state single atomic dispersion in the material
Surface, the species and component of carried metal atom can be regulated and controled as needed.
The content of the invention
The invention provides the preparation method that a kind of carbonitride loads monoatomic metal catalysis material.Prepared catalyst
Middle monometallic atom good dispersion, stability is high.The characteristics of this method has simple, easily controllable, can largely prepare nitridation
Carbon loads monoatomic metal catalysis material.
The technical solution adopted in the present invention is：A kind of carbonitride loads the preparation method of monoatomic metal catalysis material,
It is characterized in that：
(1) carbon nitrogen presoma is dissolved in solvent and solution A is made, metal precursor is dissolved in solvent solution is made
B；
(2) solution B is added in solution A, 20-150 DEG C of progress mixing 6-36h is heated under special atmosphere, so
After naturally cool to room temperature；
(3) step (2) solution removing solvent is obtained into solid metallic carbon nitrogen adduct, be ground to below 80 mesh；
(4) solid powder for obtaining step (3) is inserted in Muffle furnace or tube furnace, and line program liter is entered under special atmosphere
Warm pyrolysis processing, then naturally cools to room temperature, is ground to below 80 mesh；
(5) solid powder for obtaining step (4) is placed in Muffle furnace or tube furnace, with 10 DEG C/min under special atmosphere
Speed be heated to 450-550 DEG C, keep 1h, then naturally cool to room temperature, obtain carbonitride load monoatomic metal catalysis
Material；
Method characteristic of the present invention is：Described carbon nitrogen presoma is one in melamine, dicyandiamide, urea
Plant or two kinds of mixtures, described metal precursor is one kind in silver nitrate, silver carbonate, palladium nitrate, rhodium nitrate, platinum nitrate
Or more than two kinds, described solvent is alkalescence or neutral flux, such as water, acetonitrile, ethanol, methanol, acetone, N, N- dimethyl formyls
Amine etc., described solution A concentration is 1-500g/L, and described solution B concentration is 1-100mg/mL, described special atmosphere be
Under air, nitrogen, argon gas protective condition, described temperature programming keeps to be first heated to 300 DEG C with 1-5 DEG C/min speed
1-2h, is then heated to 400-850 DEG C with 5-10 DEG C/min speed, keeps 2-6h.
(M is Ag, Pd, Rh, Pt to the monoatomic metal M catalysis materials of lamellar graphite phase carbon nitride load prepared by the present invention
In one or two or more kinds) in metal M mass percent be 0.1-3%, metal M in zero-valent state monatomic form presence.
The present invention passes through the phase between metal center and part by the way of metal precursor and the complexing of carbon nitrogen presoma
Interaction suppresses the reunion of metallic atom, improves the stability and dispersiveness of monoatomic metal catalysis material.Process conditions letter
Single, using cheap material, reaction condition is gentle, and performance more excellent material, and preparation are obtained under relatively low preparations cost
Method has wide range of applications.Therefore, the present invention is that a kind of not only simple and efficient but also economic and environment-friendly to prepare carbonitride load monatomic
The method of metal catalytic material.
Embodiment
Embodiment 1
2g melamines are scattered in 100mL DMFs, 3h is stirred at room temperature, melamine are obtained molten
Liquid.10mg palladium nitrates are scattered in 10mL DMFs, ultrasonically treated 30min obtains palladium nitrate solution.Will
Melamine solution is transferred in 250mL round-bottomed flasks, and then 5mL palladium nitrate solutions are added in melamine solution, matched somebody with somebody
Put and be heated to 120 DEG C after condensing reflux pipe under nitrogen protective condition, lucifuge is stirred 36 hours, then naturally cools to room temperature.
Mixed solution is removed by solvent by rotary evaporation, solid metallic carbon nitrogen adduct is obtained, 24h is dried in vacuo, is then ground to
80 mesh.Solid powder is placed in ceramic crucible, is put into tube furnace, is heated under nitrogen protective condition.2 DEG C first/
Min speed is heated to 300 DEG C, keeps 2h, is then heated to 500 DEG C with 7 DEG C/min speed, keeps 2h.Natural cooling drops
Warm to room temperature, obtained solid is re-grind to 80 mesh.Finally solid powder is placed in ceramic crucible, tube furnace is put into
In, under nitrogen protective condition, 550 DEG C are heated to 10 DEG C/min speed, 1h is kept, then naturally cools to room temperature, obtain
Monoatomic metal Pd catalysis materials are loaded to carbonitride.Pd actual loading proportion is 0.51%, metal Pd in prepared material
With zero-valent state single atomic dispersion on lamellar graphite phase carbon nitride.
Embodiment 2
2g melamines are scattered in 100mL DMFs, 3h is stirred at room temperature, melamine are obtained molten
Liquid.10mg platinum nitrates are scattered in 10mL DMFs, ultrasonically treated 30min obtains platinum nitrate solution.Will
Melamine solution is transferred in 250mL round-bottomed flasks, and then 5mL platinum nitrate solutions are added in melamine solution, matched somebody with somebody
Put and be heated to 120 DEG C after condensing reflux pipe under nitrogen protective condition, lucifuge is stirred 24 hours, then naturally cools to room temperature.
Mixed solution is removed by solvent by rotary evaporation, solid metallic carbon nitrogen adduct is obtained, 24h is dried in vacuo, is then ground to
80 mesh.Solid powder is placed in ceramic crucible, is put into tube furnace, is heated under nitrogen protective condition.2 DEG C first/
Min speed is heated to 300 DEG C, keeps 2h, is then heated to 550 DEG C with 5 DEG C/min speed, keeps 4h.Natural cooling drops
Warm to room temperature, obtained solid is re-grind to 80 mesh.Finally solid powder is placed in ceramic crucible, tube furnace is put into
In, under nitrogen protective condition, 550 DEG C are heated to 10 DEG C/min speed, 1h is kept, then naturally cools to room temperature, obtain
Monoatomic metal Pt catalysis materials are loaded to carbonitride.Pt actual loading proportion is 0.47%, Pt metal in prepared material
With zero-valent state single atomic dispersion on lamellar graphite phase carbon nitride.
Embodiment 3
2g melamines are scattered in 100mL methanol, 3h is stirred at room temperature, melamine solution is obtained.By 20mg nitric acid
Silver is scattered in 10mL methanol, ultrasonically treated 30min, obtains silver nitrate solution.Melamine solution is transferred to 250mL round bottoms
In flask, then silver nitrate solution is added in melamine solution, after configuration condensing reflux pipe under nitrogen protective condition
60 DEG C are heated to, lucifuge is stirred 24 hours, then naturally cools to room temperature.Mixed solution is removed by solvent by rotary evaporation,
Solid metallic carbon nitrogen adduct is obtained, 24h is dried in vacuo, is then ground to 80 mesh.Solid powder is placed in ceramic crucible, put
Enter in tube furnace, heat under nitrogen protective condition.The speed of 1 DEG C/min first is heated to 200 DEG C, keeps 2h, then
450 DEG C are heated to 5 DEG C/min speed, 2h is kept.Natural cooling is cooled to room temperature, and obtained solid is re-grind to 80
Mesh.Finally solid powder is placed in ceramic crucible, is put into tube furnace, under nitrogen protective condition, with 10 DEG C/min speed
Rate is heated to 550 DEG C, keeps 1h, then naturally cools to room temperature, obtains carbonitride load monoatomic metal Ag catalysis materials.Institute
The actual loading proportion for preparing Ag in material is 1.89%, and metal Ag is with zero-valent state single atomic dispersion in lamellar graphite phase carbon nitride
On.
Claims (3)
1. a kind of carbonitride loads the preparation method of monoatomic metal catalysis material, it is characterised in that：
(1) carbon nitrogen presoma is dissolved in solvent and solution A is made, metal precursor is dissolved in solvent solution B is made；
(2) solution B is added in solution A, 20-150 DEG C of progress mixing 6-36h is heated under special atmosphere, then certainly
So it is cooled to room temperature；
(3) step (2) solution removing solvent is obtained into solid metallic carbon nitrogen adduct, be ground to below 80 mesh；
(4) solid powder for obtaining step (3) is inserted in Muffle furnace or tube furnace, and temperature programming heat is carried out under special atmosphere
Solution processing, then naturally cools to room temperature, is ground to below 80 mesh；
(5) solid powder for obtaining step (4) is placed in Muffle furnace or tube furnace, with 10 DEG C/min speed under special atmosphere
Rate is heated to 450-550 DEG C, keeps 1h, then naturally cools to room temperature, obtains carbonitride load monoatomic metal catalysis material.
2. according to the method described in claim 1, it is characterised in that：
Described carbon nitrogen presoma is the one or two kinds of mixture in melamine, dicyandiamide, urea；
Described metal precursor is the one or two or more kinds in silver nitrate, silver carbonate, palladium nitrate, rhodium nitrate, platinum nitrate；
Described solvent is alkalescence or neutral flux, such as water, acetonitrile, ethanol, methanol, acetone, DMF；
Described solution A concentration is 1-500g/L；
Described solution B concentration is 1-100mg/mL；
Described special atmosphere is under air, nitrogen, argon gas protective condition；
Described temperature programming keeps 1-2h to be first heated to 200-300 DEG C with 1-5 DEG C/min speed, then with 5-10 DEG C/
Min speed is heated to 400-850 DEG C, keeps 2-6h.
3. a kind of carbonitride loads the preparation method of monoatomic metal catalysis material, it is characterised in that：Lamellar graphite phase carbon nitride
Metal M quality percentage in the monoatomic metal M catalysis materials (M is the one or two or more kinds in Ag, Pd, Rh, Pt) of load
Number is 0.1-3%, and metal M exists in zero-valent state monatomic form.
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