CN109261148A - A kind of catalyst and preparation method thereof of alumina load ruthenium - Google Patents
A kind of catalyst and preparation method thereof of alumina load ruthenium Download PDFInfo
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- CN109261148A CN109261148A CN201811129657.2A CN201811129657A CN109261148A CN 109261148 A CN109261148 A CN 109261148A CN 201811129657 A CN201811129657 A CN 201811129657A CN 109261148 A CN109261148 A CN 109261148A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/462—Ruthenium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8659—Removing halogens or halogen compounds
- B01D53/8662—Organic halogen compounds
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2255/00—Catalysts
- B01D2255/10—Noble metals or compounds thereof
- B01D2255/102—Platinum group metals
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- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/209—Other metals
- B01D2255/2092—Aluminium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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Abstract
The present invention provides a kind of Ru/Al2O3Catalyst and preparation method thereof.The present invention prepares the hollow ball shape Al of nanometer sheet self assembly using hydrothermal synthesis method2O3, and noble ruthenium is supported on Al2O3On, prepare Ru/Al2O3Catalyst, wherein the mass content of ruthenium is Al2O3The 1~2% of quality, and keep Al2O3Hollow ball shape structure.Ru/Al provided by the invention2O3The ruthenium-oxide of catalyst surface can activate volatile organic matter containing chlorine in the chlorine species of catalyst surface Dissociative, have a high catalytic activity, and the Al of unique texture2O3The stability of ruthenium nano particle can be kept at high temperature, so that catalyst keeps high stability.Ru/Al of the invention2O3Industrialized production may be implemented in the preparation of catalyst, there is very high application value.
Description
Technical field
The invention belongs to environmental catalysis fields, more particularly to a kind of alumina load noble metal catalyst and its preparation
Method relates more specifically to a kind of catalyst and preparation method thereof of alumina load ruthenium.
Background technique
One of pollutant as atmosphere, volatility organic contamination compound (VOCs) attract attention, especially
It is volatile organic contaminant containing chlorine (CVOCs), because of its special stable chemical property and strong carcinogenic toxicity, large-scale application
It causes to seriously affect to environment without reasonable discharge beyond standards afterwards.To improve air quality, many environmental protection policies are to CVOCs's
It uses and discharge has strict requirements.In many end treatment means, catalytic oxidation technologies can be in low concentration, low temperature, low
Cost, it is without secondary pollution under conditions of realize elimination to CVOCs.Therefore, design has catalytic activity high and stablizes with preparation
The good catalyst of property is most important.
Most common method be Pt, Pd, Ru, Au isoreactivity component are supported on some oxides, molecular sieve or
On the carriers such as perovskite, common oxide carrier is Al2O3、CeO2、TiO2、SiO2、 ZrO2Deng.Studies have shown that noble metal is urged
Agent shows excellent catalytic activity in CVOCs catalysis burning, has to C-C key, c h bond, C-O key and C-Cl key
There is higher activation capacity, while to reaction product CO2There is good catalytic selectivity with HCl.
R.W.van den Brink et al. [Applied Catalysis B:Environmental, 1998,16 (3):
219-226] have studied Pt/ γ-Al2O3Chlorobenzene catalyst combustion reaction on catalyst.The result shows that 2%Pt/ γ-Al2O3It is right
Chlorobenzene catalysis burning has very high activity, but will form more chlorine by-products；A certain amount of water energy is added and reduces more chlorine products
It generates while improving reactivity.M.Taralunga et al. [Applied Catalysis B:Environmental, 2005,
60 (3-4): 163-171] chlorobenzene catalyst combustion reaction on Pt/H-FAU5 catalyst is had studied, catalytic activity is higher than Pt/
Al2O3And Pt/SiO2.J.-M.Giraudon et al. [Catalysis Today, 2008,137 (2-4): 379-384] has studied
Pd/ is mesoporous, macropore carrier (ZrO2、TiO2) maturing temperature and carrier must influence chlorobenzene catalyst combustion reaction on catalyst.Knot
Fruit shows the Pd/TiO of 400 DEG C of roastings2Catalyst has highest reactivity, main cause TiO2Carrier has better
Oxygen mobility.J.-F.Lamonier et al. [Catalysis Today, 2011,164 (1), 566-570] studies bis- groups of Ti-Zr
Carrier of the part as Pd catalyst, compared to the ZrO of one-component2Or TiO2Carrier has higher thermal stability.Q.G. Dai et al.
[Applied Catalysis B:Environmental, 2012,126:64-75] has studied chlorobenzene on Ru/CeO2 catalyst
Catalyst combustion reaction.The result shows that 1%Ru/CeO2Catalyst for chlorobenzene catalyst combustion reaction show excellent activity and
Stability, at a temperature of 275 DEG C, conversion ratio is greater than 95% and remains above 80h, and main cause is that Ru component has preferably
Deacon reactivity can will be adsorbed on the Cl on catalyst activity position with Cl2Form transfer.C.D.Pina et al. [Gold
Bulletin.2007,40 (1): 67- 72] Au/CeO is had studied2、Au/ZrO2、Au/Ce0.5Zr0.5O2、Au/TiO2、Au/Fe2O3
Chlorobenzene catalyst combustion reaction on catalyst.The result shows that the T of all Au catalyst50(the Au/ all within the scope of 350-400 DEG C
CeO2The activity of catalyst is best).S.Albonetti et al. is [Applied Catalysis A.2010,372 (2): 138-
146] Au/FeOx/TiO is had studied2Dichloro-benzenes catalyst combustion reaction on catalyst.The result shows that having a large amount of on Au catalyst
More chlorine by-products generate, and the deactivation phenomenom of catalyst still remains.Cl species limit very big to the poisoning effect of Au species
Application of the Au in CVOCs is made.
The catalytic oxidation activity of the catalyst of above-mentioned prior art preparation is excellent, but has the disadvantage in that catalysis reaction
Process is easy to generate more chlorine by-products, so that noble metal active component causes deactivation phenomenom because of chlorine absorption poisoning, causes to urge
The thermal stability of agent is bad.
Summary of the invention
For the deficiencies in the prior art, the purpose of the present invention is to provide a kind of catalysis of alumina load ruthenium
Agent and preparation method thereof, prepared catalyst have excellent catalytic activity and stability, can be used for industry and volatilize containing chlorine
Property catalytic organism Oxidative Degradation Process.
It illustrates: the Al in the present invention2O3For the chemistry abbreviation of aluminium oxide；Ru is the chemistry abbreviation of ruthenium； Ru/Al2O3
For the chemistry abbreviation of alumina load ruthenium.
On the one hand, the present invention provides a kind of catalyst of alumina load ruthenium, wherein the mass content of Ru is Al2O3
1~2%, Al of quality2O3For the hollow ball shape structure of nanometer sheet self assembly.
On the other hand, it the present invention provides a kind of preparation method of the catalyst of alumina load ruthenium, specifically includes as follows
Step:
(1) aluminium presoma, auxiliary agent and slow release precipitator are dissolved in deionized water, stirring obtains for 1 hour after mixing
Solution A；
(2) step (1) resulting solution A is poured into the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), by reaction kettle
Crystallization 3 hours, obtain sediment B under the conditions of being placed on 180 DEG C；
(3) sediment B that step (2) obtains is filtered and is washed to neutrality, it is 2 hours dry at 100 DEG C,
It is roasted 3 hours in 400 DEG C of air atmosphere, obtains solid C；
(4) ruthenium trichloride is added in ethyl alcohol, obtains mixed solution D after mixing evenly, take the mixed solution of 100ml
The solid C 1g that step (3) obtain is added, after ultrasonic disperse is uniform, after being spin-dried for solvent at 70 DEG C, by what is obtained in D thereto
Solid E roasts 3 hours in 500~700 DEG C of air atmosphere after 100 DEG C 2 hours dry to get the Ru/ is arrived
Al2O3Catalyst.
Aluminium presoma in the step (1) is one of aluminium chloride, aluminum nitrate and aluminum acetate；In the step (1)
The content of aluminium presoma in solution A is calculated as 0.04~0.06 mol/L by aluminum ions molar concentration.
Preferably, the aluminium presoma in the step (1) is aluminum nitrate, and the content of the aluminum nitrate is rubbed by aluminum ions
You are calculated as 0.05mol/L at concentration.
Auxiliary agent in the step (1) is one or both of potassium sulfate or sodium tartrate；It is molten in the step (1)
The molar concentration of auxiliary agent is 0.04~0.06mol/L in liquid A.
Preferably, the auxiliary agent in the step (1) is the mixture of potassium sulfate and sodium tartrate, wherein potassium sulfate and wine
The molar ratio of stone acid sodium is 4:1, and the molar concentration of the auxiliary agent is 0.05mol/L.
Slow release precipitator is a kind of in urea, ammonium carbonate and ammonium hydrogen carbonate in the step (1)；In the step (1)
The molar concentration of slow release precipitator is 0.08~0.12mol/L in solution A.
Preferably, the slow release precipitator in the step (1) is urea, and the molar concentration of the urea is 0.10mol/
L。
The content of ruthenium trichloride in the step (4) in solution D, 0.1 is calculated as by the mass concentration of ruthenium ion~
0.2mg/mL。
Preferably, the content of the ruthenium trichloride in the step (4) in solution D, is calculated as by the mass concentration of ruthenium ion
1.5mg/mL。
The present invention has following gain effect:
(1) the Ru species of the catalyst surface of alumina load ruthenium provided by the invention can activate volatility containing chlorine and have
Machine object is in the Cl species of catalyst surface Dissociative, and the Ru species of high degree of dispersion can increase catalytic activity, so that catalyst
Keep high activity.
(2) the hollow ball shape Al of multilayer chip2O3The nano particle size of noble metal Ru can be kept, catalyst performance is kept
The stabilization of energy.
(3) it will be loaded using infusion process, and select aluminium oxide as substrate carrier, there is industrial applications basis, Ke Yishi
Catalysis oxidation of the existing industrialized production cellular catalyst for the volatile organic matter containing chlorine eliminates application.
(4) chlorine volatile organic matter complete oxidation will be contained under low reaction temperatures for hydrogen chloride, carbon dioxide and water, no
The bigger more chlorine by-products of toxicity are generated, then carry out absorbing hydrogen chloride with lye, realize that volatile organic matter containing chlorine is pollution-free
Discharge.
Detailed description of the invention
Fig. 1 is the Al in embodiment 12O3The scanning electron microscope (SEM) photograph of carrier；
Fig. 2 is the Al in embodiment 12O3The nitrogen adsorption desorption figure of carrier.
Specific embodiment
The present invention is described in detail combined with specific embodiments below, but is in no way intended to limit protection scope of the present invention.
A kind of alumina support of embodiment 1
A kind of carrying alumina preparation, specifically comprises the following steps:
(1) aluminium presoma, auxiliary agent and slow release precipitator are dissolved in deionized water, stirring obtains for 1 hour after mixing
Solution A；
(2) step (1) resulting solution A is poured into the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), by reaction kettle
Crystallization 3 hours, obtain sediment B under the conditions of being placed on 180 DEG C；
(3) sediment B that step (2) obtains is filtered and is washed to neutrality, it is 2 hours dry at 100 DEG C,
It is roasted 3 hours in 400 DEG C of air atmosphere, obtains solid C to get the Al is arrived2O3Carrier.
Aluminium presoma in step (1) is aluminum nitrate, and the content of the aluminum nitrate is calculated as by aluminum ions molar concentration
0.05mol/L。
Auxiliary agent in step (1) is the mixture of potassium sulfate and sodium tartrate, wherein potassium sulfate and sodium tartrate rub
, than being 4:1, the molar concentration of the auxiliary agent is 0.05mol/L for you.
The concentration of slow release precipitator in step (1) is urea, and the molar concentration of the urea is 0.10 mol/L.
Al prepared by embodiment 12O3The surface topography of carrier is as shown in Figure 1, nitrogen adsorption desorption curve is as shown in Figure 2.
A kind of alumina support of embodiment 2
A kind of Al2O3Support preparation method, the specific steps are the same as those in embodiment 1, with embodiment 1 the difference is that:
Aluminium presoma in step (1) is aluminum acetate, and the content of the aluminum acetate is calculated as by aluminum ions molar concentration
0.06mol/L。
Auxiliary agent in step (1) is sodium tartrate, and the molar concentration of the sodium tartrate is 0.04mol/L.
The concentration of slow release precipitator in step (1) is ammonium hydrogen carbonate, and the molar concentration of the ammonium hydrogen carbonate is
0.12mol/L。
A kind of alumina support of embodiment 3
A kind of Al2O3Support preparation method, the specific steps are the same as those in embodiment 1, with embodiment 1 the difference is that:
Aluminium presoma in step (1) is aluminium chloride, and the content of the aluminium chloride is calculated as by aluminum ions molar concentration
0.04mol/L。
Auxiliary agent in step (1) is potassium sulfate, and the molar concentration of the potassium sulfate is 0.06mol/L.
The concentration of slow release precipitator in step (1) is ammonium carbonate, and the molar concentration of the ammonium carbonate is 0.08 mol/L.
A kind of catalyst of the alumina load ruthenium of embodiment 4
A kind of Ru/Al2O3Method for preparing catalyst, wherein the mass content of Ru is Al2O3The 1.5% of quality, it is specific to wrap
Include following steps:
Ruthenium trichloride is added in ethyl alcohol, obtains mixed solution D after mixing evenly, takes the mixed solution D of 100ml, to
The solid C 1g that step (3) obtains in embodiment 1 is wherein added, it, will after being spin-dried for solvent at 70 DEG C after ultrasonic disperse is uniform
Obtained solid E roasts 3 hours in 500 DEG C of air atmosphere after 100 DEG C 2 hours dry to get the Ru/ is arrived
Al2O3Catalyst.
The wherein content of the ruthenium trichloride in solution D is calculated as 0.15mg/mL by the mass concentration of ruthenium ion.
A kind of catalyst of the alumina load ruthenium of embodiment 5
A kind of Ru/Al2O3Method for preparing catalyst, wherein the mass content of Ru is Al2O3The 1% of quality, specific steps
With embodiment 4, with embodiment 4 the difference is that:
The content of ruthenium trichloride in solution D is calculated as 0.1mg/mL by the mass concentration of ruthenium ion.
A kind of catalyst of the alumina load ruthenium of embodiment 6
A kind of Ru/Al2O3Method for preparing catalyst, wherein the mass content of Ru is Al2O3The 2% of quality, specific steps
With embodiment 4, with embodiment 4 the difference is that:
The content of ruthenium trichloride in solution D is calculated as 0.2mg/mL by the mass concentration of ruthenium ion.
A kind of catalyst of the alumina load ruthenium of embodiment 7
A kind of Ru/Al2O3Method for preparing catalyst, wherein the mass content of Ru is Al2O3The 1.5% of quality, it is specific to walk
Suddenly with embodiment 4, with embodiment 4 the difference is that:
By obtained solid E after 100 DEG C 2 hours dry, roasted 3 hours in 600 DEG C of air atmosphere.
A kind of catalyst of the alumina load ruthenium of embodiment 8
A kind of Ru/Al2O3Method for preparing catalyst, wherein the mass content of Ru is Al2O3The 1.5% of quality, it is specific to walk
Suddenly with embodiment 4, with embodiment 4 the difference is that:
By obtained solid E after 100 DEG C 2 hours dry, roasted 3 hours in 700 DEG C of air atmosphere.
A kind of alumina support of comparative example 1.
Preparation method is substantially with embodiment 1, with embodiment 1 the difference is that step (1) is added without auxiliary agent.
A kind of catalyst of the alumina load ruthenium of comparative example 2
Wherein, the mass content of Ru is Al2O3The 1.5% of quality, difference of the specific steps with embodiment 4, with embodiment 4
It is:
The mixed solution D of 100ml is taken, commercialization Al is added thereto2O3Solid C 1g.
Application examples 1
By in the catalyst difference quartz ampoule fixed bed reactors in 0.1 gram of embodiment 1-5, it is in vinyl chloride concentration
1000ppm, carrier are air, total gas flow rate 50mL/min, reaction velocity are 30,000 mL/hgcatWith the item of normal pressure
Vinyl chloride catalytic oxidation is carried out under part, reaction end gas is detected with capillary gaschromatography instrument.
The catalyst that following table is 4-8 of the embodiment of the present invention and comparative example 2 provides converts during catalysis oxidation vinyl chloride
Rate corresponding conversion temperature at 90%, is denoted as T90, and measure the catalyst being prepared in embodiment 1-8 and comparative example 1-2
Specific surface area, as a result as shown in the table.
The Al prepared from embodiment 1-32O3Carrier, it can be seen that when auxiliary agent be potassium sulfate and sodium tartrate mixture,
In, when the molar ratio of potassium sulfate and sodium tartrate is 4:1, the Al of preparation2O3The specific surface area of carrier is maximum.
From embodiment 4-6 as can be seen that the content of noble ruthenium with catalyst activity be not it is proportional, with
Bullion content increases, and catalytic activity reduces.
From embodiment 4,7,8 as can be seen that when bullion content is consistent, with the raising of maturing temperature, catalysis is lived
Property decline
Comparative example 1 and comparative example 1 can not form nanometer sheet self assembly it is found that do not add auxiliary agent during the preparation process
Hollow ball shape structure so that the specific surface area of its catalyst reduces.
Comparative example 4 with comparative example 2 it is found that when bullion content it is identical, commercialized Al2O3Due to not having nanometer
The hollow ball shape structure of piece self assembly leads to the reduction of its specific surface area, and noble ruthenium oxide is uneven in its Dispersion on surface,
So as to cause catalytic activity reduction.
As seen from the above table, catalyst prepared by embodiment 4-8 has excellent catalytic activity, wherein in embodiment 4
T90It is 355 DEG C.
Only as described above, is only a preferred embodiment of the present invention, when the model that cannot limit implementation of the invention with this
It encloses, i.e., generally according to simple equivalent changes and modifications made by content documented by the claims in the present invention and description of the invention,
All it is still covered by the claims of the invention.It is searched in addition, abstract part and title are intended merely to auxiliary patent document
It seeks and being used, the interest field being not intended to limit the invention.
Claims (7)
1. a kind of catalyst of alumina load ruthenium, it is characterised in that: the mass content of Ru is Al2O31~2%, Al of quality2O3
For the hollow ball shape structure of nanometer sheet self assembly.
2. the preparation method of the catalyst of alumina load ruthenium as described in claim 1, it is characterised in that: specifically include as follows
Step:
(1) aluminium presoma, auxiliary agent and slow release precipitator are dissolved in deionized water, stirring obtains solution in 1 hour after mixing
A；
(2) step (1) resulting solution A is poured into the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), reaction kettle is placed on
Crystallization 3 hours, obtain sediment B under the conditions of 180 DEG C；
(3) sediment B that step (2) obtains is filtered and is washed to neutrality, it is 2 hours dry at 100 DEG C, at 400 DEG C
Air atmosphere in roast 3 hours, obtain solid C；
(4) ruthenium trichloride is added in ethyl alcohol, obtains mixed solution D after mixing evenly, take the mixed solution D, Xiang Qi of 100ml
The middle solid C 1g that step (3) are added and obtain, after ultrasonic disperse is uniform, after being spin-dried for solvent at 70 DEG C, obtained solid E is existed
100 DEG C after drying 2 hours, 3 hours are roasted in 500~700 DEG C of air atmosphere to get to the alumina load ruthenium
Catalyst.
3. the preparation method of the catalyst of alumina load ruthenium as claimed in claim 2, it is characterised in that: the step (1)
In aluminium presoma be one of aluminium chloride, aluminum nitrate and aluminum acetate；Aluminium presoma contains in solution A in the step (1)
Amount, is calculated as 0.04~0.06mol/L by aluminum ions molar concentration.
4. the preparation method of the catalyst of alumina load ruthenium as claimed in claim 2, it is characterised in that: the step (1)
In auxiliary agent be one or both of potassium sulfate and sodium tartrate；The molar concentration of auxiliary agent is in solution A in the step (1)
0.04~0.06mol/L.
5. the preparation method of the catalyst of alumina load ruthenium as claimed in claim 2, it is characterised in that: the step (1)
Middle slow release precipitator is one of urea, ammonium carbonate and ammonium hydrogen carbonate；Slow release precipitator in solution A in the step (1)
Molar concentration be 0.08~0.12mol/L.
6. the preparation method of the catalyst of alumina load ruthenium as claimed in claim 2, it is characterised in that: the step (4)
The content of ruthenium trichloride in middle solution D is calculated as 0.1~0.2mg/mL by the mass concentration of ruthenium ion.
7. application of the catalyst of alumina load ruthenium as described in claim 1 in catalysis oxidation vinyl chloride.
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| CN114849701A (en) * | 2022-06-01 | 2022-08-05 | 北京化工大学 | Hollow spherical catalyst for fixed bed with particle internal fluidization and preparation method thereof |
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Application publication date: 20190125 |