CN109939712A - A kind of monatomic noble metal catalyst and its preparation and the application in room temperature catalytic oxidation formaldehyde - Google Patents
A kind of monatomic noble metal catalyst and its preparation and the application in room temperature catalytic oxidation formaldehyde Download PDFInfo
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- CN109939712A CN109939712A CN201910200405.2A CN201910200405A CN109939712A CN 109939712 A CN109939712 A CN 109939712A CN 201910200405 A CN201910200405 A CN 201910200405A CN 109939712 A CN109939712 A CN 109939712A
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Abstract
The present invention relates to a kind of monatomic noble metal catalysts and its preparation and the application in room temperature catalytic oxidation formaldehyde, the catalyst to be prepared by the following method: (1) by after activated carbon modified processing, being impregnated in precious metal salt solution, obtain maceration extract;(2) under ultra-low temperature surroundings, reducing agent solution is mixed with the maceration extract in step (1), is reacted;(3) reactant of step (2) is filtered, washed and is dried, the monatomic noble metal catalyst of support type is made.This method is simple and environmentally-friendly, and the noble metal in catalyst obtained is dispersed in metal oxide surface with monatomic form, and the content of noble metal is 0.01-0.3wt%, is used in the reaction of room temperature catalytic oxidation formaldehyde, formaldehyde removal rate is up to 93% or more.
Description
Technical field
The invention belongs to catalyst to synthesize field, and in particular to a kind of monatomic noble metal catalyst and its preparation and in room
Application in warm catalysis oxidation formaldehyde.
Background technique
The formaldehyde that house decorative material is discharged is one of the important indoor pollutant for threatening human health, there is carcinogenic work
With especially bigger to the toxic action of newborn, child, the elderly.Therefore of crucial importance for the removal of formaldehyde.Activity at present
Charcoal absorption is a kind of common method of purifying formaldehyde, but active carbon is easier to absorption non-polar compound, PARA FORMALDEHYDE PRILLS(91,95) isopolarity molecule
Adsorption effect is poor.And the hole of active carbon may also be blocked by some impurity and seriously affect adsorption effect.In addition, conduct
It mainly include noble metal and base metal two major classes except the catalytic oxidation of one of formaldehyde ideal method.Noble metal catalyst compared with
Base metal has the characteristic of better low-temperature catalytic oxidation formaldehyde, but its higher cost.Therefore, it should guarantee precious metal catalyst
The using effect of agent reduces usage amount save the cost again.The noble metal catalyst particle for many methods preparation reported at present
For nano-scale, precious metal atom utilization rate is low, and room temperature degradation effect is poor.
Summary of the invention
Based on the above issues, an object of the present invention is to provide a kind of preparation method of monatomic noble metal catalyst,
This method is simple and environmentally-friendly, and atom fraction is presented in monatomic noble metal catalyst obtained, active component noble metal on the activated carbon
It dissipates.
To achieve the goals above, technical scheme is as follows:
A kind of preparation method of monatomic noble metal catalyst, includes the following steps:
(1) it by after activated carbon modified processing, is impregnated in precious metal salt solution, obtains maceration extract;
(2) under ultra-low temperature surroundings, reducing agent solution is mixed with the maceration extract in step (1), is reacted;
(3) reactant of step (2) is filtered, washed and is dried, the monatomic noble metal of support type is made and urges
Agent.
Preferably, the step (1) specifically comprises the following steps:
Active carbon after the processing of the modified solution of nitrogenous compound, is impregnated in precious metal salt solution, is obtained by (1a)
Maceration extract.
Preferably, in step (1a), active carbon immersion treatment 3-10h in the modified solution at 20-120 DEG C.
Preferably, in step (1a), the mass fraction of the modified solution is 1%-30%.
Preferably, in step (1a), the nitrogenous compound is glutamic acid, glycine, urea, dimethylamine, p-aminophenyl
Formic acid, nitromethane, any one or more in nitrophenol.
There is no particular limitation for the solvent of modified solution described in step (1a), can be as known to those skilled in the art
Conventional solvents, preferably water.
The quality of active carbon described in step (1a) and modified solution is not particularly limited, and meeting active carbon can be complete
It is immersed in modified solution entirely.
Preferably, in step (1) and (1a), the active carbon impregnates 8-12h in precious metal salt solution.
Preferably, in step (1) and (1a), the dipping is to carry out under stiring, and the rate of stirring is 300-1000r/
min。
Preferably, in step (1) and (1a), the concentration of the precious metal salt solution is 0.0004-0.01mol/L.
The quality of precious metal salt described in step (1) and (1a) and active carbon does not limit, and meets and to be prepared
The content of noble metal is 0.01-0.3wt% in the noble metal of single atomic dispersion.
The solvent of noble metal precursor liquid solution described in step (1) and (1a) is noncondensing anti-freeze-thaw under ultra-low temperature surroundings
Any one or more in agent, preferably water or alcohols, more preferably water, ethyl alcohol, any one or more in ethylene glycol.
Preferably, in step (1) and (1a), the precious metal salt is the chloride and/or nitrate of noble metal, described
Noble metal is preferably any one or more in Au, Ag, Pt, Pd.
Preferably, in step (2), the mixing/reaction carries out under stiring, and the rate of stirring is 300-1000r/
min;Reaction time is 2-6h.
Preferably, in step (2), the molar ratio of the reducing agent and noble metal is 5:1-100:1;The reducing agent solution
Concentration be 0.01-0.1mol/L, avoid reacting violent progress.
In step (2), the solvent of the reducing agent solution is noncondensing anti-freeze solvent, preferably water under ultra-low temperature surroundings
Or any one or more in alcohols, more preferably water, ethyl alcohol, any one or more in ethylene glycol.
Preferably, in step (2), the reducing agent is hydrazine hydrate, sodium borohydride, potassium borohydride, ascorbic acid, lemon
Sour sodium, sodium sulfite, any one or more in potassium sulfite.
Preferably, in step (3), filtering and washing carries out under ultralow temperature.
Preferably, in step (3), the temperature of the drying process is 60-100 DEG C;The time of the drying process is 12-
24h。
Above-mentioned ultralow temperature is -80 to 0 DEG C
It the second object of the present invention is to provide a kind of monatomic noble metal catalyst, is prepared by the above method
It arrives.
Preferably, the noble metal is dispersed in metal oxide surface with monatomic form, and the content of noble metal is 0.01-
0.3wt%, in terms of catalyst full dose.
The third object of the present invention is to provide a kind of application of monatomic noble metal catalyst, is by above method system
For what is obtained, can be used in the reaction of room temperature catalytic oxidation formaldehyde.
Beneficial effects of the present invention:
The preparation method of the monatomic noble metal catalyst of support type of the invention, this method is simple and environmentally-friendly, and active carbon passes through
Modification introduces nitrogenous compound, enhances the interaction between carrier active carbon and noble metal, improves noble metal in work
Dispersion on property charcoal;Meanwhile ultralow reaction temperature can effectively inhibit metal nucleation, to improve monodispersed precious metal atom
Concentration, makes the content 0.01-0.3wt% of noble metal active component, and carrier surface is highly dispersed in the form of monatomic, real
Existing 100% atom utilization.The catalyst is used in the reaction of room temperature catalytic oxidation formaldehyde, shows high formaldehyde at room temperature
Degradation efficiency, removal rate are up to 93% or more.
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) it by after activated carbon modified processing, is impregnated in precious metal salt solution, obtains maceration extract;
(2) under ultra-low temperature surroundings, reducing agent solution is mixed with the maceration extract in step (1), is reacted;
(3) reactant of step (2) is filtered, washed and is dried, the monatomic noble metal of support type is made and urges
Agent.
Preferably, the step (1) specifically comprises the following steps:
Active carbon after the processing of the modified solution of nitrogenous compound, is impregnated in precious metal salt solution, is obtained by (1a)
Maceration extract.
Preferably, in step (1a), active carbon immersion treatment 3-10h in the modified solution at 20-120 DEG C.
Preferably, in step (1a), the mass fraction of the modified solution is 1%-30%.
Preferably, in step (1a), the nitrogenous compound is glutamic acid, glycine, urea, dimethylamine, p-aminophenyl
Formic acid, nitromethane, any one or more in nitrophenol.
There is no particular limitation for the solvent of modified solution described in step (1a), can be as known to those skilled in the art
Conventional solvents, preferably water.
The quality of active carbon described in step (1a) and modified solution is not particularly limited, and meeting active carbon can be complete
It is immersed in modified solution entirely.
Preferably, in step (1) and (1a), the active carbon impregnates 8-12h in precious metal salt solution, for example, 8,9,
10、11、12h。
In step (1) and (1a), the dipping can use the ancillary measure of those skilled in the art's routine, for example, can
It is carried out in ultrasound or stirring, or the combination of ultrasound or stirring two ways, can also be the recycling of aforesaid way.
Preferably, in step (1) and (1a), the dipping is to carry out under stiring, and the rate of stirring is 300-1000r/
Min, for example, 300,400,500,600,700,800,900,1000r/min.
Preferably, in step (1) and (1a), the concentration of the precious metal salt solution is 0.0004-0.01mol/L, such as
For 0.0004,0.001,0.02,0.003,0.004,0.005,0.06,0.007,0.008,0.009,0.01mol/L.
The quality of precious metal salt described in step (1) and (1a) and active carbon does not limit, and meets and to be prepared
In the noble metal of single atomic dispersion the content of noble metal be 0.01-0.3wt%, for example, 0.01,0.05,0.1,0.15,0.2,
0.25,0.3wt%.
The solvent of noble metal precursor liquid solution described in step (1) and (1a) is noncondensing anti-freeze-thaw under ultra-low temperature surroundings
Any one or more in agent, preferably water or alcohols, more preferably water, ethyl alcohol, any one or more in ethylene glycol.
Preferably, in step (1) and (1a), the precious metal salt is the chloride and/or nitrate of noble metal, described
Noble metal is preferably any one or more in Au, Ag, Pt, Pd, for example, PdCl2、Pd(NO3)2、Na2PdCl4、HAuCl4﹒
3H2O、H2PtCl6﹒ 6H2O、Pt(NO3)2, any one or more in AgNO3.
Those skilled in the art knows, selects different noble metal precursor bodies that different noble metals can be prepared and urges
Agent;Noble metal in the noble metal catalyst can be used as single noble metal, also can be used as two or more noble metals.Make
Be it is preferred, synthesize noble metal Au catalyst when select HAuCl4 ﹒ 3H2O as noble metal precursor body.Synthesize precious metals pt catalyst
When select H2PtCl6 ﹒ 6H2O or Pt (NO3) 2 as noble metal precursor body.PdCl2, Pd are selected when synthesizing precious metals pd catalyst
(NO3) 2 or Na2PdCl4 is as noble metal precursor body.Those skilled in the art knows, to preparation containing two or more expensive
When the catalyst of metal, corresponding noble metal precursor body is selected.
In step (2), there is no particular limitation for the mixed mode, is conventional hand as known to those skilled in the art
Section and method, such as reducing agent can be added drop-wise in maceration extract or directly reducing agent is added in maceration extract.
Preferably, in step (2), the mixing/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 2-6h, for example, 2,3,4,5,
6h。
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;The concentration of the reducing agent solution be 0.01-0.1mol/L, for example, 0.01,0.02,0.03,
0.04,0.05,0.06,0.07,0.08,0.09,0.1mol/L, avoid reacting violent progress.
In step (2), the solvent of the reducing agent solution is noncondensing anti-freeze solvent, preferably water under ultra-low temperature surroundings
Or any one or more in alcohols, more preferably water, ethyl alcohol, any one or more in ethylene glycol.
Preferably, in step (2), the reducing agent is hydrazine hydrate, sodium borohydride, potassium borohydride, ascorbic acid, lemon
Sour sodium, sodium sulfite, any one or more in potassium sulfite.
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 under ultralow temperature.
Preferably, in step (3), the temperature of the drying process is 60-100 DEG C, for example, 60,70,80,90,100
℃;The time of the drying process be 12-24h, for example, 12,15,18,20, for 24 hours.
Above-mentioned ultralow temperature is -80 to 0 DEG C, for example, -80, -70, -60, -50, -40, -30, -20, -10,0 DEG C.
The monatomic noble metal catalyst being prepared by the above method, the noble metal are dispersed in monatomic form
The content of metal oxide surface, noble metal is 0.01-0.3wt%, in terms of catalyst full dose.
Above-mentioned monatomic noble metal catalyst can be used in the reaction of room temperature catalytic oxidation formaldehyde.
Monatomic noble metal catalyst made from the above method can be used in the reaction of room temperature catalytic oxidation formaldehyde, test environment
Temperature is 25 DEG C, relative humidity 40Rh.It weighs 20g catalyst to be put in 1.5 cubes of standard aldehyde test cabins, using Dongguan ring
Instrument equipment Co., Ltd HY-JQ-1 generator discharges pollution sources formaldehyde, is monitored using Britain recordable type methylene oxide detecting instrument PPM-HTV
Concentration of formaldehyde in cabin, initial concentration 1-1.2mg/m3, for 24 hours after formaldehyde removal rate up to 93% or more.
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
It is spare that active carbon is dried to 12h in 105 DEG C of drying box.10g active carbon is weighed, 20mL mass fraction, which is added, is
2% glutamic acid solution stands 3h after shaken at room temperature 1h, filters off maceration extract, dry at 105 DEG C, obtains modified activated carbon.
Configure 20mL 0.003mol/L H2PtCl6﹒ 6H2O solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;Room
10g modified activated carbon is added to H under temperature2PtCl6﹒ 6H2In O solution, stirring dipping 8h, stirring rate 500rmp;It prepares
60mL 0.01mol/L hydrazine hydrate solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;By H2PtCl6﹒ 6H2O solution and water
It closes hydrazine solution to be respectively put into low-temp reaction case, when temperature is reduced to -60 DEG C, hydrazine hydrate solution is slowly added into
H2PtCl6﹒ 6H2In O solution, low-temp reaction 3h;It washs after reaction, dry, it is that 0.1% monatomic is urged that Pt content, which is made,
Agent.The catalyst is used in formaldehyde room temperature Degrading experiment, initial concentration of formaldehyde 1mg/m3, concentration of formaldehyde is afterwards for 24 hours
0.018mg/m3, formaldehyde removal rate is 98.2%.
Embodiment 2
It is spare that active carbon is dried to 12h in 105 DEG C of drying box.10g active carbon is weighed, 20mL mass fraction, which is added, is
5% glycine solution stands 8h after shaken at room temperature 1h, filters off maceration extract, dry at 105 DEG C, obtains modified activated carbon.
Configure 20mL0.003mol/L H2PtCl6﹒ 6H2O solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;Room temperature
It is lower that 10g modified activated carbon is added to H2PtCl6﹒ 6H2In O solution, stirring dipping 8h, stirring rate 500rmp;Prepare 60mL
0.01mol/L hydrazine hydrate solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;By H2PtCl6﹒ 6H2O solution and hydrazine hydrate are molten
Liquid is respectively put into low-temp reaction case, and when temperature is reduced to -60 DEG C, hydrazine hydrate solution is slowly added into H2PtCl6﹒ 6H2O
In solution, low-temp reaction 3h;It washs after reaction, it is dry, the monatomic catalyst that Pt content is 0.1% is made.The catalysis
Agent is used in formaldehyde room temperature Degrading experiment, initial concentration of formaldehyde 1.2mg/m3, rear concentration of formaldehyde is 0.0576mg/m for 24 hours3, first
Aldehyde removal rate is 95.2%.
Embodiment 3
It is spare that active carbon is dried to 12h in 105 DEG C of drying box.10g active carbon is weighed, 20mL volume fraction, which is added, is
30% nitrophenol solution stands 10h after shaken at room temperature 1h, filters off maceration extract, dry at 105 DEG C, obtains modified active
Charcoal.
Configure 20mL0.01mol/L AgNO3Solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;At room temperature by 10g
Modified activated carbon is added to AgNO3In solution, stirring dipping 8h, stirring rate 500rmp;Prepare 20mL 0.1mol/L hydration
Hydrazine solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;By AgNO3Solution and hydrazine hydrate solution are respectively put into low-temp reaction
In case, when temperature is reduced to -60 DEG C, hydrazine hydrate solution is slowly added into AgNO3In solution, low-temp reaction 3h;Reaction knot
It is washed after beam, it is dry, the monatomic catalyst that Ag content is 0.2% is made.The catalyst is used in formaldehyde room temperature Degrading experiment,
Initial concentration of formaldehyde is 1mg/m3, rear concentration of formaldehyde is 0.064mg/m for 24 hours3, formaldehyde removal rate is 93.6%.
Embodiment 4
It is spare that active carbon is dried to 12h in 105 DEG C of drying box.10g active carbon is weighed, 20mL mass fraction, which is added, is
5% urea liquid stands 8h after shaken at room temperature 1h, filters off maceration extract, dry at 105 DEG C, obtains modified activated carbon.
Configure 20mL0.003mol/L H2PtCl6﹒ 6H2O solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;Room temperature
It is lower that 10g modified activated carbon is added to H2PtCl6﹒ 6H2In O solution, stirring dipping 8h, stirring rate 500rmp;Prepare 60mL
0.01mol/L sodium borohydride solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;By H2PtCl6﹒ 6H2O solution and hydroboration
Sodium solution is respectively put into low-temp reaction case, and when temperature is reduced to -60 DEG C, sodium borohydride solution is slowly added into
H2PtCl6﹒ 6H2In O solution, low-temp reaction 3h;It washs after reaction, dry, it is that 0.1% monatomic is urged that Pt content, which is made,
Agent.The catalyst is used in formaldehyde room temperature Degrading experiment, initial concentration of formaldehyde 1mg/m3, concentration of formaldehyde is afterwards for 24 hours
0.022mg/m3, formaldehyde removal rate is 97.8%.
Embodiment 5
It is spare that active carbon is dried to 12h in 105 DEG C of drying box.10g active carbon is weighed, 20mL mass fraction, which is added, is
10% dimethylamine solution stands 8h after shaken at room temperature 1h, filters off maceration extract, dry at 105 DEG C, obtains modified activated carbon.
Configure 20mL0.005mol/L Pd (NO3)2Solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;At room temperature will
10g modified activated carbon is added to Pd (NO3)2In solution, stirring dipping 8h, stirring rate 500rmp;Prepare 10mL 0.1mol/
L hydrazine hydrate solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;By Pd (NO3)2Solution and hydrazine hydrate solution are respectively put into low
In warm reaction chamber, when temperature is reduced to -60 DEG C, hydrazine hydrate solution is slowly added into Pd (NO3)2In solution, low-temp reaction
3h;It washs after reaction, it is dry, the monatomic catalyst that Pd content is 0.1% is made.The catalyst is dropped for formaldehyde room temperature
In solution test, initial concentration of formaldehyde 1mg/m3, rear concentration of formaldehyde is 0.068mg/m for 24 hours3, formaldehyde removal rate is 93.2%.
Embodiment 6
It is spare that active carbon is dried to 12h in 105 DEG C of drying box.10g active carbon is weighed, 20mL mass fraction, which is added, is
10% p-aminobenzoic acid solution stands 8h after shaken at room temperature 1h, filters off maceration extract, dry at 105 DEG C, obtains modified work
Property charcoal.
Configure 20mL0.005mol/L HAuCl4﹒ 3H2O solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;Room temperature
It is lower that 10g modified activated carbon is added to HAuCl4﹒ 3H2In O solution, stirring dipping 8h, stirring rate 500rmp;Prepare 10mL
0.1mol/L hydrazine hydrate solution, by water and ethyl alcohol, 1:9 is formed solvent by volume;By HAuCl4﹒ 3H2O solution and hydrazine hydrate solution
It is respectively put into low-temp reaction case, when temperature is reduced to -60 DEG C, hydrazine hydrate solution is slowly added into HAuCl4﹒ 3H2O solution
In, low-temp reaction 3h;It washs after reaction, it is dry, the monatomic catalyst that Au content is 0.2% is made.The catalyst is used
In formaldehyde room temperature Degrading experiment, initial concentration of formaldehyde 1.2mg/m3, rear concentration of formaldehyde is 0.0476mg/m for 24 hours3, formaldehyde goes
Except rate is 96.0%.
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 monatomic noble metal catalyst, which comprises the steps of:
(1) it by after activated carbon modified processing, is impregnated in precious metal salt solution, obtains maceration extract;
(2) under ultra-low temperature surroundings, reducing agent solution is mixed with the maceration extract in step (1), is reacted;
(3) reactant of step (2) is filtered, washed and is dried, monatomic noble metal catalyst is made.
2. preparation method according to claim 1, which is characterized in that the activated carbon modified processing specifically includes following step
It is rapid: active carbon is handled by the modified solution of nitrogenous compound.
3. preparation method according to claim 2, which is characterized in that the mass fraction of the modified solution is 1%-
30%.
4. preparation method according to claim 2, which is characterized in that the nitrogenous compound is glutamic acid, glycine, urine
Element, dimethylamine, p-aminobenzoic acid, nitromethane, any one or more in nitrophenol.
5. preparation method according to any one of claims 1-4, which is characterized in that precious metal salt described in step (1)
The concentration of solution is 0.0004-0.01mol/L;The molar ratio of the reducing agent and noble metal is 5:1-100:1;The reducing agent
The concentration of solution is 0.01-1mol/L.
6. preparation method described in -5 any one according to claim 1, which is characterized in that the precious metal salt is noble metal
Chloride and/or nitrate;The reducing agent is hydrazine hydrate, sodium borohydride, potassium borohydride, ascorbic acid, sodium citrate, sulfurous
Any one or more in sour sodium, potassium sulfite;The solvent of the precious metal salt solution and reducing agent solution is ultralow temperature ring
Noncondensing anti-freeze solvent under border.
7. preparation method described in -6 any one according to claim 1, which is characterized in that the ultralow temperature is -80 to 0 DEG C;
Reaction time is 2-6h.
8. a kind of monatomic noble metal catalyst, which is characterized in that the monatomic noble metal catalyst according to claim 1-7
Method described in any one is prepared.
9. monatomic noble metal catalyst according to claim 8, which is characterized in that the noble metal is with monatomic form
It is dispersed in activated carbon surface, the content 0.01-0.3wt% of noble metal, in terms of catalyst full dose.
10. the application of monatomic noble metal catalyst according to claim 8 or claim 9, which is characterized in that described monatomic expensive
Metallic catalyst is in the reaction of room temperature catalytic oxidation formaldehyde.
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