CN110026186A - A kind of monatomic catalyst of metal of activated carbon from activated sludge load and its preparation and application - Google Patents
A kind of monatomic catalyst of metal of activated carbon from activated sludge load and its preparation and application Download PDFInfo
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Abstract
The present invention relates to a kind of monatomic catalyst of metal of activated carbon from activated sludge load and its preparation and application, the catalyst to be prepared by the following method: activated carbon from activated sludge being mixed with metal front liquid solution, obtains suspension；Under low temperature and illumination condition, reducing agent reduction is added in above-mentioned suspension, filters, washs, it is dry, obtain the monatomic catalyst of metal of activated carbon from activated sludge load.This method is fast and convenient, equipment is simple, raw material is easy to get, it is low in cost, it is environmental friendly, it is easy to industrialize, the characteristics of monatomic catalyst of the metal of preparation shows high load amount, high activity, high stability, high dispersive, in it can be applicable to catalytic degradation VOCs reaction and cinnamic acid cortex cinnamomi hydrogenation reaction, high VOCs removal rate and high catalytic activity are shown.
Description
Technical field
The invention belongs to waste resource utilization and catalyst preparation technical fields, and in particular to a kind of activated carbon from activated sludge is negative
The monatomic catalyst of the metal of load and preparation and application.
Background technique
Biological carbon based material is concerned as a kind of efficient, green, multi-functional electrode material.Biomass type is numerous
More, cheap, substantial amounts and widely distributed, and advantageously form flourishing microcellular structure are prepare charcoal high-quality
Material.The advantages that obtained Carbon Materials are in broken shape, and compact structure, ash content is lower, strong adsorption, low in cost.
Monatomic catalyst is the forward position direction of current catalytic science research, and monatomic catalyst has highest original
Sub- utilization rate, high activity and highly selective, have become current hot spot.The synthesis monatomic catalyst of load type metal faces
Main challenge is: how to make to be formed it is monatomic evenly dispersed while avoid metallic atom from reuniting.Synthesis is negative at present
The main method of the monatomic catalyst of load type includes mass-selected soft-landing technology, wet chemistry method and original
Sublayer sedimentation.Mass-selected soft-landing technology can be accurately controlled the particle size of carried metal, atom
Layer sedimentation, which may be implemented in, uniformly deposits single metal atom on high specific surface area porous carrier, however maintains this two technologies
What is run is costly, is unfavorable for its application in actually synthesis.The experimental provision of wet chemistry synthetic method is easy, common
Chemical laboratory can be completed, but this method monoatomic metal dispersibility is difficult to control, and is not suitable for synthesis high load amount
Monatomic catalyst.
The present invention proposes a kind of monatomic noble metal catalyst and preparation method thereof of activated carbon from activated sludge load, the biology
Matter is living to be used as carrier, not only improves the utilization rate of biomass energy, and reduce catalyst cost, and by carrying out chemistry under low temperature also
Former and photo-reduction, prepares the monatomic catalyst of metal of high load amount, high activity, high stability, high dispersive.And the preparation
Method is fast and convenient, environmental protection, low in cost, is easy to industrialize, have a good application prospect in catalytic field.
Summary of the invention
Based on the above issues, the metal that an object of the present invention is to provide a kind of load of activated carbon from activated sludge monatomic is urged
The preparation method of agent, this method is fast and convenient, and equipment is simple, and raw material is easy to get, low in cost, environmental friendly, is easy to industrialize,
The characteristics of monatomic catalyst of the metal of preparation shows high load amount, high activity, high stability, high dispersive.
To achieve the goals above, technical scheme is as follows:
A kind of preparation method of the monatomic catalyst of metal of activated carbon from activated sludge load, includes the following steps:
(1) activated carbon from activated sludge is mixed with metal front liquid solution, obtains suspension；
(2) under low temperature and illumination condition, reducing agent reduction is added in the suspension of step (1), filters, washs, does
It is dry, obtain the monatomic catalyst of metal of activated carbon from activated sludge load.
Preferably, activated carbon from activated sludge described in step (1) includes the following steps: by being activated at 60-80 DEG C
Under, by nitric acid solution spray on activated carbon from activated sludge.
Preferably, the mass fraction of the nitric acid solution is 10-60%, and the flow velocity of nitric acid spray is 5-20mL/min.
Preferably, activated carbon from activated sludge described in step (1) is cocoanut active charcoal, active fruit shell carbon, wood activated charcoal.
Preferably, the concentration of metal front liquid solution described in step (1) is 0.001-0.1mol/L.
Preferably, metal precursor described in step (1) is the chloride and/or nitrate of metal, and the metal is preferred
For platinum, palladium, rhodium, ruthenium, gold is silver-colored, osmium, any one or more in iridium.
Preferably, the illumination in the step (2) is ultraviolet light irradiation.
Preferably, the recovery time described in step (2) is 10-30min.
Preferably, the molar ratio of reducing agent described in step (2) and noble metal is 5:1-100:1.
Preferably, reducing agent described in step (2) is hydrazine hydrate, sodium borohydride, potassium sulfite, appointing in ascorbic acid
It anticipates one or more.
Preferably, filtering and washing described in step (3) carries out at low temperature.
Preferably, the temperature of drying process described in step (3) is 20-50 DEG C；The time of the drying process is 12-
24h。
Above-mentioned low temperature is -40 to 0 DEG C
It is to pass through the second object of the present invention is to provide a kind of monatomic catalyst of metal of activated carbon from activated sludge load
The above method is prepared.
Preferably, the metal is dispersed in biomass active carbon surface with monatomic form, and the content of metal is 0.1-
2wt%, in terms of catalyst full dose.
The third object of the present invention is to provide a kind of application of the monatomic catalyst of metal of activated carbon from activated sludge load,
It is to be prepared by the above method, can be applicable in catalytic degradation VOCs reaction.
Preferably, the reaction condition of the catalytic degradation VOCs are as follows: reaction temperature is 20-25 DEG C, relative humidity 30-
50Rh。
The fourth object of the present invention is to provide a kind of application of the monatomic catalyst of metal of activated carbon from activated sludge load,
It is to be prepared by the above method, can be applicable in hydrogenation on cinnamic aldehyde reaction.
Preferably, the cinnamic acid cortex cinnamomi adds the reaction condition of hydrogen are as follows: and under hydrogen atmosphere, reaction temperature is 50-100 DEG C,
Reaction pressure is 1-5MPa.
Beneficial effects of the present invention:
The monatomic catalyst of metal of the invention not only improves the utilization of biomass energy using activated carbon from activated sludge as carrier
Rate, and reduce catalyst cost；Ultralow reaction temperature can effectively inhibit metal nucleation, so that it is former to improve monodispersed noble metal
Sub- concentration；Electronation and photo-reduction combine, and not only can quickly prepare monoatomic metal, but also make the metal on carrier
High degree of dispersion while reduction, will not reunite；The monatomic catalyst of the metal of preparation shows high load amount, high activity, height
The characteristics of stability, high dispersive, in the dry state, after six months, catalytic performance does not change yet.
In one embodiment of the invention, activated carbon from activated sludge is N doping based biomass active carbon, surface official containing N
Can roll into a ball can preferably be entrained in Carbon Materials with metal, strong interaction can occur with metal, further increase catalyst
Load capacity, activity, stability and dispersibility.
The monatomic catalyst of metal of the invention shows high VOCs removal rate, VOCs in room temperature degradation VOCs reaction
Removal rate is up to 90% or more.It is living that the monatomic catalyst of metal of the invention shows high catalysis in hydrogenation on cinnamic aldehyde reaction
Property, the conversion ratio of cinnamic acid is up to 95% or more, and the selectivity of cinnamyl alcohol is up to 98% or more.
The preparation method of the monatomic catalyst of metal of the invention have it is fast and convenient, equipment is simple, and raw material is easy to get, cost
It is cheap, it is environmental friendly, it is easy to industrialized feature, the monatomic catalyst of the metal of preparation shows high load amount, high activity, height
The characteristics of stability, high dispersive.
Detailed description of the invention:
Fig. 1 is the transmission electron microscope picture of monatomic catalyst.
Specific embodiment:
Combined with specific embodiments below, the present invention is described in more detail.
A kind of preparation method of monatomic noble metal catalyst, includes the following steps:
(1) activated carbon from activated sludge is mixed with metal front liquid solution, obtains suspension；
(2) under low temperature and illumination condition, reducing agent reduction is added in the suspension of step (1), filters, washs, does
It is dry, obtain the monatomic catalyst of metal of activated carbon from activated sludge load.
Preferably, activated carbon from activated sludge described in step (1) is cocoanut active charcoal, active fruit shell carbon, wood activated charcoal.
Preferably, activated carbon from activated sludge described in step (1) includes the following steps: by activation processing at 60-80 DEG C,
At for example, 60,70,80 DEG C, by nitric acid solution spray on activated carbon from activated sludge.
Preferably, the mass fraction of the nitric acid solution is 10-60%, for example, 10,20,30,40,50,60%, nitric acid
The flow velocity of spray is 5-20mL/min, for example, 5mL/min, 10mL/min, 15mL/min, 20mL/min.
There is no particular limitation for the solvent of the nitric acid solution, can be Conventional solvents as known to those skilled in the art,
Preferably water.
The quality of activated carbon from activated sludge described in step (1) and nitric acid solution is not particularly limited, and it is molten to meet nitric acid
Liquid can be sprayed uniformly in biomass active carbon surface.
In step (1), the mixing can use the ancillary measure of those skilled in the art's routine, for example, can be in ultrasound
Or carried out in stirring, or the combination of ultrasound or stirring two ways, it can also be the recycling of aforesaid way.
Preferably, in step (1), the mixing is to carry out under stiring, and the rate of stirring is 300-1000r/min, example
For example 300,400,500,600,700,800,900,1000r/min.
Preferably, in step (1), the concentration of the precious metal salt solution is 0.001-0.1mol/L, for example, 0.001,
0.005、 0.008、0.01、0.02、0.03、0.05、0.08、0.09、0.1mol/L。
Metal precursor described in step (1) and the quality of activated carbon from activated sludge do not limit, and satisfaction is prepared
Single atomic dispersion noble metal in noble metal content be 0.1-2wt%, for example, 0.1,0.5,1,1.5,2wt%.
The solvent of metal front liquid solution described in step (1) is noncondensing anti-freeze solvent under ultra-low temperature surroundings, preferably
For any one or more in water or alcohols, more preferably water, ethyl alcohol, any one or more in ethylene glycol.
Preferably, in step (1), the metal precursor is the chloride and/or nitrate of metal, and the metal is preferred
For platinum, palladium, rhodium, ruthenium, gold is silver-colored, osmium, any one or more in iridium, for example, chloroplatinic acid, platinum nitrate, palladium chloride, chlorine palladium acid
Sodium, palladium nitrate, radium chloride, rhodium nitrate, ruthenic chloride, gold chloride, silver nitrate, chloro-iridic acid, potassium osmate are any one in chlorine osmic acid ammonium
Kind is a variety of.
Those skilled in the art knows, selects different metal precursors that different metal catalytics can be prepared
Agent；Metal in the metallic catalyst can be used as single metal, also can be used as two or more metals.
Preferably, the illumination in the step (2) is ultraviolet light irradiation.
Preferably, in step (2), the reduction reaction carries out under stiring, and the rate of stirring is 300-1000r/
Min, for example, 300,400,500,600,700,800,900,1000r/min；Reaction time is 10-30min, for example, 10,
20、30min。
Preferably, in step (2), the molar ratio of the reducing agent and noble metal is 5:1-100:1, for example, 5:1,10:
1、 20:1、50:1、100:1。
Preferably, in step (2), the reducing agent is hydrazine hydrate, sodium borohydride, potassium sulfite, in ascorbic acid
Any one or more.
It is described to be filtered, washed and dried treatment process there is no particular limitation in step (3), it is those skilled in the art
The conventional means and method that member knows.
Preferably, in step (3), filtering and washing carries out at low temperature.
Preferably, in step (3), the temperature of the drying process is 20-50 DEG C, for example, 20,30,40,50 DEG C；It is described
The time of drying process be 12-24h, for example, 12,15,18,20, for 24 hours.
Above-mentioned low temperature is -40 to 0 DEG C, for example, -40, -30, -20, -10,0 DEG C.
By the monoatomic metal catalyst for the activated carbon from activated sludge load that the above method is prepared, the metal is with list
Atomic form is dispersed in biomass active carbon surface, and the content of metal is 0.1-2wt%, in terms of catalyst full dose.
The monoatomic metal catalyst of above-mentioned activated carbon from activated sludge load is in catalytic degradation VOCs reaction.
Catalytic degradation VOCs reaction condition are as follows: reaction temperature is 20-25 DEG C, relative humidity 30-50Rh, concrete operations
Are as follows: it weighs 20g catalyst and is placed in 1.5m3 code test cabin, temperature is 20-25 DEG C in cabin, and relative humidity 30-50Rh is adopted
Pollution sources VOCs is discharged with Dongguan Huan Yi equipment Co., Ltd HY-JQ-1 generator, using the auspicious portable PGM-7340 of China, the U.S.
VOCs concentration in type VOCs detector test cabin, initial concentration 3-5mg/m3, for 24 hours after remaining VOCs concentration in test chamber.
The monoatomic metal catalyst of above-mentioned activated carbon from activated sludge load is in hydrogenation on cinnamic aldehyde reaction.
Cortex cinnamomi hydrogenation conditions are as follows: under hydrogen atmosphere, reaction temperature is 50-100 DEG C, reaction pressure 1-5MPa, tool
Gymnastics conduct: weighing 20-50mg catalyst and be placed in 50mL autoclave, adds the cinnamic acid and 5-15mL of 2-5mmol
Isopropanol, with hydrogen displacement be filled with hydrogen afterwards several times to 1-5MPa, in 50-100 DEG C of reaction 2-5h.It is cooled to after the reaction was completed
Room temperature, centrifuging and taking supernatant liquor are analyzed.Product analysis uses the GC-2014C type gas-chromatography of Japanese Shimadzu.
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
10g cocoanut active charcoal is weighed, carries out spray process with the aqueous solution of nitric acid of 10wt%, the flow velocity of nitric acid spray is
5mL/min is heated while spray, and heating temperature is 60 DEG C.After the completion of spray, continue to spray with deionized water
Cleaning 3 times.(Pd load capacity is 0.1wt% to the chlorine palladium acid sodium solution of active carbon and 0.001mol/L that processing is completed, and solvent is
Water) it is mixed to get suspension, it is placed in high-low temperature chamber, sodium borohydride (sodium borohydride: Pd is added when temperature is down to -40 DEG C
=5:1, molar ratio), while being irradiated with ultraviolet lamp, low temperature filtering and washing after 20min, monatomic Pd/ is made in drying at room temperature
Pd/carbon catalyst.
Above-mentioned catalyst is used in catalytic degradation VOCs reaction, concrete operations are as follows: weigh 20g catalyst and be placed in 1.5m3
In code test cabin, temperature is 25 DEG C, relative humidity 30Rh in cabin, and initial VOCs concentration is 3mg/m3, for 24 hours in rear test chamber
Remaining VOCs concentration is0.5mg/m3。
Above-mentioned catalyst is used in hydrogenation on cinnamic aldehyde reaction, concrete operations are as follows: weigh 50mg catalyst and be placed in 50mL high
It presses in reaction kettle, adds the cinnamic acid of 5mmol and the isopropanol of 15mL, Hydrogen Vapor Pressure 2MPa, 80 DEG C of reaction 2h.It has reacted
It is cooled to room temperature after, centrifuging and taking supernatant liquor is analyzed, and the conversion ratio of cinnamic acid is 96.6%, and the selectivity of cinnamyl alcohol is
98.1%.
Embodiment 2
10g active fruit shell carbon is weighed, carries out spray process with the aqueous solution of nitric acid of 60wt%, the flow velocity of nitric acid spray is
20mL/min is heated while spray, and heating temperature is 80 DEG C.After the completion of spray, continue to spray with deionized water
Leaching cleaning 3 times.(Pd load capacity is 2wt% to the platinum nitrate solution of active carbon and 0.1mol/L that processing is completed, and solvent is second
Alcohol) it is mixed to get suspension, it is placed in high-low temperature chamber, ascorbic acid (ascorbic acid: Pt=is added when temperature is down to 0 DEG C
100:1, molar ratio), while being irradiated with ultraviolet lamp, low temperature filtering and washing after 20min, monatomic Pt/ is made in drying at room temperature
Pd/carbon catalyst.
Above-mentioned catalyst is used in catalytic degradation VOCs reaction, concrete operations are as follows: weigh 20g catalyst and be placed in 1.5m3
In code test cabin, temperature is 25 DEG C, relative humidity 30Rh in cabin, and initial VOCs concentration is 3mg/m3, for 24 hours in rear test chamber
Remaining VOCs concentration is0.2mg/m3。
Above-mentioned catalyst is used in hydrogenation on cinnamic aldehyde reaction, concrete operations are as follows: weigh 50mg catalyst and be placed in 50mL high
It presses in reaction kettle, adds the cinnamic acid of 5mmol and the isopropanol of 15mL, Hydrogen Vapor Pressure 2MPa, 80 DEG C of reaction 2h.It has reacted
It is cooled to room temperature after, centrifuging and taking supernatant liquor is analyzed, and the conversion ratio of cinnamic acid is 98.3%, and the selectivity of cinnamyl alcohol is
99.3%.
Embodiment 3
10g wood activated charcoal is weighed, carries out spray process with the aqueous solution of nitric acid of 30wt%, the flow velocity of nitric acid spray is
10mL/min is heated while spray, and heating temperature is 60 DEG C.After the completion of spray, continue to spray with deionized water
Leaching cleaning 3 times.(Pd load capacity is 2wt% to the rhodium nitrate solution of active carbon and 0.1mol/L that processing is completed, and solvent is second two
Alcohol) it is mixed to get suspension, it is placed in high-low temperature chamber, ascorbic acid (ascorbic acid: Pd is added when temperature is down to -40 DEG C
=100:1, molar ratio), while being irradiated with ultraviolet lamp, low temperature filtering and washing after 20min, drying at room temperature is made monatomic
Rh/ Pd/carbon catalyst.
Above-mentioned catalyst is used in catalytic degradation VOCs reaction, concrete operations are as follows: weigh 20g catalyst and be placed in 1.5m3
In code test cabin, temperature is 25 DEG C, relative humidity 30Rh in cabin, and initial VOCs concentration is 3mg/m3, for 24 hours in rear test chamber
Remaining VOCs concentration is0.3mg/m3。
Above-mentioned catalyst is used in hydrogenation on cinnamic aldehyde reaction, concrete operations are as follows: weigh 50mg catalyst and be placed in 50mL high
It presses in reaction kettle, adds the cinnamic acid of 5mmol and the isopropanol of 15mL, Hydrogen Vapor Pressure 2MPa, 80 DEG C of reaction 2h.It has reacted
It is cooled to room temperature after, centrifuging and taking supernatant liquor is analyzed, and the conversion ratio of cinnamic acid is 97.8%, and the selectivity of cinnamyl alcohol is
98.3%.
Embodiment 4
10g cocoanut active charcoal is weighed, carries out spray process with the aqueous solution of nitric acid of 30wt%, the flow velocity of nitric acid spray is
10mL/min is heated while spray, and heating temperature is 60 DEG C.After the completion of spray, continue to spray with deionized water
Leaching cleaning 3 times.(Ru load capacity is 2wt% to the chlorination ruthenium solution of active carbon and 0.1mol/L that processing is completed, and solvent is second two
Alcohol) it is mixed to get suspension, it is placed in high-low temperature chamber, ascorbic acid (ascorbic acid: Ru is added when temperature is down to -40 DEG C
=100:1, molar ratio), while being irradiated with ultraviolet lamp, low temperature filtering and washing after 20min, drying at room temperature is made monatomic
Ru/ Pd/carbon catalyst.
Above-mentioned catalyst is used in catalytic degradation VOCs reaction, concrete operations are as follows: weigh 20g catalyst and be placed in 1.5m3
In code test cabin, temperature is 25 DEG C, relative humidity 30Rh in cabin, and initial VOCs concentration is 3mg/m3, for 24 hours in rear test chamber
Remaining VOCs concentration is0.32mg/m3。
Above-mentioned catalyst is used in hydrogenation on cinnamic aldehyde reaction, concrete operations are as follows: weigh 50mg catalyst and be placed in 50mL high
It presses in reaction kettle, adds the cinnamic acid of 5mmol and the isopropanol of 15mL, Hydrogen Vapor Pressure 2MPa, 80 DEG C of reaction 2h.It has reacted
It is cooled to room temperature after, centrifuging and taking supernatant liquor is analyzed, and the conversion ratio of cinnamic acid is 97.4%, and the selectivity of cinnamyl alcohol is
98.1%.
Embodiment 5
10g cocoanut active charcoal is weighed, carries out spray process with the aqueous solution of nitric acid of 30wt%, the flow velocity of nitric acid spray is
10mL/min is heated while spray, and heating temperature is 60 DEG C.After the completion of spray, continue to spray with deionized water
Leaching cleaning 3 times.(Ir load capacity is 2wt% to the Chloroiridic Acid solution of active carbon and 0.1mol/L that processing is completed, and solvent is second two
Alcohol) it is mixed to get suspension, it is placed in high-low temperature chamber, potassium sulfite (potassium sulfite: Ir is added when temperature is down to -40 DEG C
=100:1, molar ratio), while being irradiated with ultraviolet lamp, low temperature filtering and washing after 20min, drying at room temperature is made monatomic
Ir/ Pd/carbon catalyst.
Above-mentioned catalyst is used in catalytic degradation VOCs reaction, concrete operations are as follows: weigh 20g catalyst and be placed in 1.5m3
In code test cabin, temperature is 25 DEG C, relative humidity 30Rh in cabin, and initial VOCs concentration is 3mg/m3, for 24 hours in rear test chamber
Remaining VOCs concentration is0.33mg/m3。
Above-mentioned catalyst is used in hydrogenation on cinnamic aldehyde reaction, concrete operations are as follows: weigh 50mg catalyst and be placed in 50mL high
It presses in reaction kettle, adds the cinnamic acid of 5mmol and the isopropanol of 15mL, Hydrogen Vapor Pressure 2MPa, 80 DEG C of reaction 2h.It has reacted
It is cooled to room temperature after, centrifuging and taking supernatant liquor is analyzed, and the conversion ratio of cinnamic acid is 97.1%, and the selectivity of cinnamyl alcohol is
98.2%.
Embodiment 6
10g cocoanut active charcoal is weighed, carries out spray process with the aqueous solution of nitric acid of 30wt%, the flow velocity of nitric acid spray is
10mL/min is heated while spray, and heating temperature is 60 DEG C.After the completion of spray, continue to spray with deionized water
Leaching cleaning 3 times.(Os load capacity is 2wt% to the chlorine osmic acid ammonium salt solution of active carbon and 0.1mol/L that processing is completed, and solvent is second
Glycol) be mixed to get suspension, be placed in high-low temperature chamber, when temperature is down to -40 DEG C be added sodium borohydride (sodium borohydride:
Os=100:1, molar ratio), while being irradiated with ultraviolet lamp, low temperature filtering and washing after 20min, drying at room temperature, it is made single former
Sub- Os/ Pd/carbon catalyst.
Above-mentioned catalyst is used in catalytic degradation VOCs reaction, concrete operations are as follows: weigh 20g catalyst and be placed in 1.5m3
In code test cabin, temperature is 25 DEG C, relative humidity 30Rh in cabin, and initial VOCs concentration is 3mg/m3, for 24 hours in rear test chamber
Remaining VOCs concentration is0.35mg/m3。
Above-mentioned catalyst is used in hydrogenation on cinnamic aldehyde reaction, concrete operations are as follows: weigh 50mg catalyst and be placed in 50mL high
It presses in reaction kettle, adds the cinnamic acid of 5mmol and the isopropanol of 15mL, Hydrogen Vapor Pressure 2MPa, 80 DEG C of reaction 2h.It has reacted
It is cooled to room temperature after, centrifuging and taking supernatant liquor is analyzed, and the conversion ratio of cinnamic acid is 97.2%, and the selectivity of cinnamyl alcohol is
97.8%.
Embodiment 7
10g cocoanut active charcoal is weighed, carries out spray process with the aqueous solution of nitric acid of 30wt%, the flow velocity of nitric acid spray is
10mL/min is heated while spray, and heating temperature is 60 DEG C.After the completion of spray, continue to spray with deionized water
Leaching cleaning 3 times.By the chlorauric acid solution of the chlorine palladium acid sodium and 0.05mol/L of the active carbon of processing completion and 0.05mol/L, (Pd is negative
Carrying capacity is 1wt%, and Au load capacity is 1wt%, and solvent is that water and ethyl alcohol are formed according to volume ratio 2:8) it is mixed to get suspension,
It is placed in high-low temperature chamber, hydrazine hydrate (hydrazine hydrate: Pd=100:1, molar ratio) is added when temperature is down to -40 DEG C, uses simultaneously
Ultraviolet lamp is irradiated, low temperature filtering and washing after 30min, drying at room temperature, and monatomic Au/Pd/ Pd/carbon catalyst is made.
Above-mentioned catalyst is used in catalytic degradation VOCs reaction, concrete operations are as follows: weigh 20g catalyst and be placed in 1.5m3
In code test cabin, temperature is 25 DEG C, relative humidity 30Rh in cabin, and initial VOCs concentration is 3mg/m3, for 24 hours in rear test chamber
Remaining VOCs concentration is0.1mg/m3。
Above-mentioned catalyst is used in hydrogenation on cinnamic aldehyde reaction, concrete operations are as follows: weigh 50mg catalyst and be placed in 50mL high
It presses in reaction kettle, adds the cinnamic acid of 5mmol and the isopropanol of 15mL, Hydrogen Vapor Pressure 2MPa, 80 DEG C of reaction 2h.It has reacted
It is cooled to room temperature after, centrifuging and taking supernatant liquor is analyzed, and the conversion ratio of cinnamic acid is 98.8%, and the selectivity of cinnamyl alcohol is
99.6%.
Transmission electron microscope observing is scanned to the monatomic catalyst of embodiment 1-7, obtained scanning transmission electron microscope photo
It is similar to Fig. 1, show that metallic atom is highly dispersed at carrier surface with single atomic form, soilless sticking phenomenon occurs.
Technical solution of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint
What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the monatomic catalyst of metal of activated carbon from activated sludge load, which is characterized in that including walking as follows
It is rapid:
(1) activated carbon from activated sludge is mixed with metal front liquid solution, obtains suspension；
(2) under low temperature and illumination condition, reducing agent reduction is added in the suspension of step (1), filters, washs, it is dry, it obtains
The monatomic catalyst of metal loaded to activated carbon from activated sludge.
2. preparation method according to claim 1, which is characterized in that activated carbon from activated sludge described in step (1) is through making a living
Change processing, includes the following steps: at 60-80 DEG C, by nitric acid solution spray on activated carbon from activated sludge.
3. preparation method according to claim 1, which is characterized in that activated carbon from activated sludge described in step (1) is coconut husk
Active carbon, active fruit shell carbon, wood activated charcoal.
4. preparation method according to claim 1, which is characterized in that metal precursor described in step (1) is metal
Chloride and/or nitrate, the metal are platinum, and palladium, rhodium, ruthenium, gold is silver-colored, osmium, any one or more in iridium；Step (2)
Described in reducing agent be hydrazine hydrate, sodium borohydride, potassium sulfite, any one or more in ascorbic acid.
5. preparation method according to claim 1, which is characterized in that the illumination in the step (2) is ultraviolet light irradiation.
6. preparation method according to claim 1, which is characterized in that the recovery time described in step (2) is 10-30min.
7. preparation method according to claim 1, which is characterized in that the low temperature is -40 to 0 DEG C.
8. the metal of the load of activated carbon from activated sludge made from preparation method described in -7 any one is monatomic according to claim 1
Catalyst, which is characterized in that the metal is dispersed in biomass active carbon surface with monatomic form, and the content of metal is 0.1-
2wt%, in terms of catalyst full dose.
9. the application of the monatomic catalyst of metal of activated carbon from activated sludge load according to claim 8, which is characterized in that
The catalyst is applied in catalytic degradation VOCs reaction.
10. the application of the monatomic catalyst of metal of activated carbon from activated sludge load according to claim 8, feature exist
In the catalyst is applied in hydrogenation on cinnamic aldehyde reaction.
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Application publication date: 20190719 |