CN107649123A - A kind of preparation method of alumina-coated noble metal catalyst - Google Patents
A kind of preparation method of alumina-coated noble metal catalyst Download PDFInfo
- Publication number
- CN107649123A CN107649123A CN201711049881.6A CN201711049881A CN107649123A CN 107649123 A CN107649123 A CN 107649123A CN 201711049881 A CN201711049881 A CN 201711049881A CN 107649123 A CN107649123 A CN 107649123A
- Authority
- CN
- China
- Prior art keywords
- reaction
- noble metal
- preparation
- alumina
- metal catalyst
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 56
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 65
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 53
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000007789 sealing Methods 0.000 claims abstract description 30
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 26
- 238000003825 pressing Methods 0.000 claims abstract description 18
- 239000012141 concentrate Substances 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 16
- 150000003983 crown ethers Chemical class 0.000 claims abstract description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 15
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 235000019441 ethanol Nutrition 0.000 claims abstract description 8
- 238000003801 milling Methods 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 235000013339 cereals Nutrition 0.000 claims description 5
- 235000013312 flour Nutrition 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000012495 reaction gas Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000013467 fragmentation Methods 0.000 abstract description 3
- 238000006062 fragmentation reaction Methods 0.000 abstract description 3
- 238000002161 passivation Methods 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 12
- 239000003345 natural gas Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- -1 platinum ion Chemical class 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 235000007926 Craterellus fallax Nutrition 0.000 description 1
- 240000007175 Datura inoxia Species 0.000 description 1
- 229910016978 MnOx Inorganic materials 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013384 organic framework Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J23/42—Platinum
-
- B01J35/50—
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention belongs to noble metal catalyst field, and in particular to a kind of preparation method of alumina-coated noble metal catalyst, using being acidified after spent auto-catalysts fragmentation, add polyvinylpyrrolidone sealing reaction and vacuum distillation reaction obtains concentrate；The sealing pressing reaction of absolute ethyl alcohol is carried out after concentrate filtering, is filtrated to get passivation platinum particles；Then it is passivated in the ethanol solution of platinum particles addition nano-aluminum hydroxide after aerated reaction to add crown ether stirring reaction and stand and reacts, obtains crystalline solid；Crystalline solid is finally subjected to sintering of milling, obtains catalyst.The present invention can play the purpose of twice laid using spent automotive exhaust catalysts as raw material, greatly reduce preparation cost.
Description
Technical field
The invention belongs to noble metal catalyst field, and in particular to a kind of preparation side of alumina-coated noble metal catalyst
Method.
Background technology
It is increasingly urgent with the energy and environmental problem, for environmental protection, the energy is saved, people are to motor-vehicle tail-gas
Emission control proposes higher requirement.Start Chinese on January 1st, 2013 to perform the discharge standard of natural gas engine state five.China
Natural gas is compared with horn of plenty, and many city buses and taxi use natural gas as fuel, plus natural gas as a kind of
Develop the energy, can also be widely used in the future in fuel for motor vehicle.Therefore, the Research on Post-processing Techniques control natural gas tailstock is strengthened
Gas discharge is imperative, is particularly important as the core component catalyst in post-processing technology.Relative to gasoline car, naturally
Gas tail gas catalyst technology is not still high in development starting stage, technology maturity.
Zhao Bin et al. (China rare earth journal, article numbering：1000-4343 (2003) -0098-03) use La-Al2O3、
La-Al2O3+CeO2-ZrO2And La-Al2O3+CeO2-ZrO2.MnOx it is carrier material, adds carrier material, helps during ball milling slurrying
The method of agent and noble metal prepares natural gas purification catalyst.This invention, noble metal are easy to from internal migration to coating surface,
Noble metal reduces phenomenon from surface to inside into concentration, and noble metal surface is excessively assembled, and loss late is high, causes catalyst performance
Difference.
Chinese patent (CN200810225539.1) is milled to certain particle size using by catalysis material, impregnates noble metal, dries
Powder is obtained after dry, roasting, then ball milling slurrying.By slurry coated on ceramic honeycomb carrier, urged after drying, roasting
Agent.The advantage of such a method is, noble metal is fixed on material with regard to load before refining, and noble metal will not move during defibrination
Move.The surface of this invention noble metal dispersion powder before non-ball milling, during defibrination, powder can be destroyed, fragmentation, be produced new disconnected
Face, and new surface does not have noble metal can not carry out catalytic action, reduces catalyst performance.
The content of the invention
For the problems of the prior art, the present invention provides a kind of preparation method of alumina-coated noble metal catalyst,
The purpose of twice laid can be played as raw material using spent automotive exhaust catalysts, greatly reduces preparation cost.
To realize above technical purpose, the technical scheme is that：A kind of system of alumina-coated noble metal catalyst
Preparation Method, it is characterised in that：The step of preparation method, is as follows：
Step 1, spent automotive exhaust catalysts are subjected to break process, then crushed using flour mill, salt is added dropwise
Acid solution, form stable suspension；
Step 2, suspension is added into polyvinylpyrrolidone, sealing reaction 2-4h, is then evaporated under reduced pressure 1-2h, obtains dense
Contracting liquid；
Step 3, white precipitate is obtained after concentrate filtering, absolute ethyl alcohol sealing pressing reaction 2-3h, mistake is added after drying
Platinum particles after being passivated after filter；
Step 4, nano-aluminum hydroxide is added into absolute ethyl alcohol, then adds platinum particles, aerated reaction 2-4h, obtain
Mixed precipitation liquid；
Step 5, crown ether is added into mixed precipitation liquid, reaction 12-24h is stirred at room temperature, until being completely dissolved, Ran Houjing
24-48h is put, is filtrated to get crystalline solid；
Step 6, sintered after crystalline solid is milled, obtain alumina-coated noble metal catalyst.
Dropwise addition hydrochloric acid speed in the step 1 is 10-15mL/min, and the suspension pH is 3-4.
Broken rear powder in the step 1 is 0.1-10 μm.
The addition of polyvinylpyrrolidone in the step 2 is the 3-8% of catalyst quality.
The temperature of sealing reaction in the step 2 is 40-60 DEG C, and the vacuum distillation temperature is 80-100 DEG C, pressure
For the 40-50% of atmospheric pressure, the volume of concentrate is the 20-25% of suspension.
The reaction solution of sealing pressing reaction in the step 3 is the ethanol that concentration is 10-15mg/L.
The temperature of sealing pressing reaction in the step 3 is 60-70 DEG C, pressure 2-5MPa.
The concentration of nano-aluminum hydroxide in the step 4 is 10-15mg/L, and platinum particles concentration is 2-8mg/L, and aeration is anti-
It is nitrogen or air to answer gas, and the flow velocity of the aerated reaction is 10-20mL/min, and aerated reaction temperature is 40-50 DEG C.
The addition of crown ether in the step 5 is 2-4 times of nano-aluminum hydroxide mole, mixing speed 1000-
1500r/min。
Sintering temperature in the step 6 is 200-400 DEG C, and the grain diameter after milling is not more than 10 microns.
Auto-exhaust catalyst is carried out break process by step 1, can catalyst breakage, being capable of shape by the way that hydrochloric acid is added dropwise
Into suspension, using the insoluble of platinum and hydrochloric acid, form insoluble matter, and the material of catalyst by dissolving with hydrochloric acid in water.
Step 2 adds polyvinylpyrrolidone in suspension and forms dispersion effect, and polyvinylpyrrolidone has good
Dispersion effect, suspended things surface can be gathered in, seal reaction and be evaporated under reduced pressure reaction it is public by way of concentrated, obtain
To the concentrate with dispersion effect.
Step 3 platinum ion scattered by polyvinylpyrrolidone is obtained after the filtered drying of concentrate, and in ethanol condition
Platinum particles surface can be passivated by lower sealing pressing reaction, and the passivation is passivated for ion.
Nano-aluminum hydroxide is added absolute ethyl alcohol and forms suspension by step 4, is then added platinum particles, is passed through aerated reaction
Nano-aluminum hydroxide and platinum particles can be mixed, and there is good toughness, polyethylene pyrrole in itself using aluminium hydroxide
Pyrrolidone, which is dissolved in absolute ethyl alcohol, forms micro- thick shape, and platinum particles are scattered wherein, and surrounding forms aluminum hydroxide precipitation.
Step 5 adds crown ether into solution, and middle crown ether is stirred at room temperature and dissolves the aluminium hydroxide containing platinum particles, shape
Into organic framework, good dissolubility is played；During long-time is stood, absolute ethyl alcohol slowly volatilizees, and crown ether is gradual
Separate out, carry out crystalline solid.
Step 6 sinters crystalline solid the platinum particles catalyst that can obtain aluminum oxide parcel after milling.
The present invention is acidified after using spent auto-catalysts fragmentation, adds polyvinylpyrrolidone sealing reaction and decompression
Distillation reaction obtains concentrate；The sealing pressing reaction of absolute ethyl alcohol is carried out after concentrate filtering, is filtrated to get passivation platinum particles；
Then platinum particles are passivated add in the ethanol solution of nano-aluminum hydroxide and crown ether stirring reaction and quiet is added after aerated reaction
Reaction is put, obtains crystalline solid；Crystalline solid is finally subjected to sintering of milling, obtains catalyst.
From the above, it can be seen that the present invention possesses advantages below：
1. the present invention can play the purpose of twice laid using spent automotive exhaust catalysts as raw material, drop significantly
Low preparation cost.
2. catalyst prepared by the present invention is used for catalytic reaction, good catalytic effect, stable performance can be played.
3. the preparation method of the present invention is simple and easy, condition is easy to control, practical.
Embodiment
Describe the present invention in detail in conjunction with the embodiments, but any restriction is not done to the claim of the present invention.
Embodiment 1
A kind of preparation method of alumina-coated noble metal catalyst, it is characterised in that：The step of preparation method, is such as
Under：
Step 1, spent automotive exhaust catalysts are subjected to break process, then crushed using flour mill, salt is added dropwise
Acid solution, form stable suspension；
Step 2, suspension is added into polyvinylpyrrolidone, sealing reaction 2h, is then evaporated under reduced pressure 1h, is concentrated
Liquid；
Step 3, white precipitate is obtained after concentrate filtering, absolute ethyl alcohol sealing pressing reaction 2h, filtering is added after drying
After be passivated after platinum particles；
Step 4, nano-aluminum hydroxide is added into absolute ethyl alcohol, then adds platinum particles, aerated reaction 2h, mixed
Close precipitated liquid；
Step 5, crown ether is added into mixed precipitation liquid, reaction 12h is stirred at room temperature, until being completely dissolved, then stands
24h, it is filtrated to get crystalline solid；
Step 6, sintered after crystalline solid is milled, obtain alumina-coated noble metal catalyst.
Dropwise addition hydrochloric acid speed in the step 1 is 10mL/min, and the suspension pH is 3.
Broken rear powder in the step 1 is 0.1 μm.
The addition of polyvinylpyrrolidone in the step 2 is the 3% of catalyst quality.
The temperature of sealing reaction in the step 2 is 40 DEG C, and the vacuum distillation temperature is 80 DEG C, and pressure is atmospheric pressure
40%, the volume of concentrate is the 20% of suspension.
The reaction solution of sealing pressing reaction in the step 3 is the ethanol that concentration is 10mg/L.
The temperature of sealing pressing reaction in the step 3 is 60 DEG C, pressure 2MPa.
The concentration of nano-aluminum hydroxide in the step 4 is 10mg/L, and platinum particles concentration is 2mg/L, aerated reaction gas
Body is nitrogen, and the flow velocity of the aerated reaction is 10mL/min, and aerated reaction temperature is 40 DEG C.
The addition of crown ether in the step 5 is 2 times of nano-aluminum hydroxide mole, mixing speed 1000r/
min。
Sintering temperature in the step 6 is 200 DEG C, and the grain diameter after milling is 10 microns.
Embodiment 2
A kind of preparation method of alumina-coated noble metal catalyst, it is characterised in that：The step of preparation method, is such as
Under：
Step 1, spent automotive exhaust catalysts are subjected to break process, then crushed using flour mill, salt is added dropwise
Acid solution, form stable suspension；
Step 2, suspension is added into polyvinylpyrrolidone, sealing reaction 4h, is then evaporated under reduced pressure 2h, is concentrated
Liquid；
Step 3, white precipitate is obtained after concentrate filtering, absolute ethyl alcohol sealing pressing reaction 3h, filtering is added after drying
After be passivated after platinum particles；
Step 4, nano-aluminum hydroxide is added into absolute ethyl alcohol, then adds platinum particles, aerated reaction 4h, mixed
Close precipitated liquid；
Step 5, crown ether is added into mixed precipitation liquid, reaction 24h is stirred at room temperature, until being completely dissolved, then stands
48h, it is filtrated to get crystalline solid；
Step 6, sintered after crystalline solid is milled, obtain alumina-coated noble metal catalyst.
Dropwise addition hydrochloric acid speed in the step 1 is 15mL/min, and the suspension pH is 4.
Broken rear powder in the step 1 is 10 μm.
The addition of polyvinylpyrrolidone in the step 2 is the 8% of catalyst quality.
The temperature of sealing reaction in the step 2 is 60 DEG C, and the vacuum distillation temperature is 100 DEG C, and pressure is air
The 50% of pressure, the volume of concentrate is the 25% of suspension.
The reaction solution of sealing pressing reaction in the step 3 is the ethanol that concentration is 15mg/L.
The temperature of sealing pressing reaction in the step 3 is 70 DEG C, pressure 5MPa.
The concentration of nano-aluminum hydroxide in the step 4 is 15mg/L, and platinum particles concentration is 8mg/L, aerated reaction gas
Body is air, and the flow velocity of the aerated reaction is 20mL/min, and aerated reaction temperature is 50 DEG C.
The addition of crown ether in the step 5 is 4 times of nano-aluminum hydroxide mole, mixing speed 1500r/
min。
Sintering temperature in the step 6 is 400 DEG C, and the grain diameter after milling is 5 microns.
Embodiment 3
A kind of preparation method of alumina-coated noble metal catalyst, it is characterised in that：The step of preparation method, is such as
Under：
Step 1, spent automotive exhaust catalysts are subjected to break process, then crushed using flour mill, salt is added dropwise
Acid solution, form stable suspension；
Step 2, suspension is added into polyvinylpyrrolidone, sealing reaction 3h, is then evaporated under reduced pressure 2h, is concentrated
Liquid；
Step 3, white precipitate is obtained after concentrate filtering, absolute ethyl alcohol sealing pressing reaction 2h, filtering is added after drying
After be passivated after platinum particles；
Step 4, nano-aluminum hydroxide is added into absolute ethyl alcohol, then adds platinum particles, aerated reaction 3h, mixed
Close precipitated liquid；
Step 5, crown ether is added into mixed precipitation liquid, reaction 18h is stirred at room temperature, until being completely dissolved, then stands
36h, it is filtrated to get crystalline solid；
Step 6, sintered after crystalline solid is milled, obtain alumina-coated noble metal catalyst.
Dropwise addition hydrochloric acid speed in the step 1 is 13mL/min, and the suspension pH is 4.
Broken rear powder in the step 1 is 3 μm.
The addition of polyvinylpyrrolidone in the step 2 is the 5% of catalyst quality.
The temperature of sealing reaction in the step 2 is 40-60 DEG C, and the vacuum distillation temperature is 90 DEG C, and pressure is big
The 45% of air pressure, the volume of concentrate are the 23% of suspension.
The reaction solution of sealing pressing reaction in the step 3 is the ethanol that concentration is 13mg/L.
The temperature of sealing pressing reaction in the step 3 is 65 DEG C, pressure 3MPa.
The concentration of nano-aluminum hydroxide in the step 4 is 12mg/L, and platinum particles concentration is 5mg/L, aerated reaction gas
Body is nitrogen, and the flow velocity of the aerated reaction is 15mL/min, and aerated reaction temperature is 45 DEG C.
The addition of crown ether in the step 5 is 3 times of nano-aluminum hydroxide mole, mixing speed 1200r/
min。
Sintering temperature in the step 6 is 300 DEG C, and the grain diameter after milling is 7 microns.
Performance detection is as follows：
Comparative example is existing noble metal catalyst.
In summary, the present invention has advantages below：
1. the present invention can play the purpose of twice laid using spent automotive exhaust catalysts as raw material, drop significantly
Low preparation cost.
2. catalyst prepared by the present invention is used for catalytic reaction, good catalytic effect, stable performance can be played.
3. the preparation method of the present invention is simple and easy, condition is easy to control, practical.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical scheme described by inventive embodiments.It will be understood by those within the art that still the present invention can be carried out
Modification or equivalent substitution, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (10)
- A kind of 1. preparation method of alumina-coated noble metal catalyst, it is characterised in that：The step of preparation method, is as follows：Step 1, spent automotive exhaust catalysts are subjected to break process, then crushed using flour mill, it is molten that hydrochloric acid is added dropwise Liquid, form stable suspension；Step 2, suspension is added into polyvinylpyrrolidone, sealing reaction 2-4h, is then evaporated under reduced pressure 1-2h, is concentrated Liquid；Step 3, white precipitate is obtained after concentrate filtering, absolute ethyl alcohol sealing pressing reaction 2-3h is added after drying, after filtering Platinum particles after being passivated；Step 4, nano-aluminum hydroxide is added into absolute ethyl alcohol, then adds platinum particles, aerated reaction 2-4h, mixed Precipitated liquid；Step 5, crown ether is added into mixed precipitation liquid, reaction 12-24h is stirred at room temperature, until being completely dissolved, then stands 24-48h, it is filtrated to get crystalline solid；Step 6, sintered after crystalline solid is milled, obtain alumina-coated noble metal catalyst.
- A kind of 2. preparation method of alumina-coated noble metal catalyst according to claim 1, it is characterised in that：It is described Dropwise addition hydrochloric acid speed in step 1 is 10-15mL/min, and the suspension pH is 3-4.
- A kind of 3. preparation method of alumina-coated noble metal catalyst according to claim 1, it is characterised in that：It is described Broken rear powder in step 1 is 0.1-10 μm.
- A kind of 4. preparation method of alumina-coated noble metal catalyst according to claim 1, it is characterised in that：It is described The addition of polyvinylpyrrolidone in step 2 is the 3-8% of catalyst quality.
- A kind of 5. preparation method of alumina-coated noble metal catalyst according to claim 1, it is characterised in that：It is described The temperature of sealing reaction in step 2 is 40-60 DEG C, and the vacuum distillation temperature is 80-100 DEG C, and pressure is the 40- of atmospheric pressure 50%, the volume of concentrate is the 20-25% of suspension.
- A kind of 6. preparation method of alumina-coated noble metal catalyst according to claim 1, it is characterised in that：It is described The reaction solution of sealing pressing reaction in step 3 is the ethanol that concentration is 10-15mg/L.
- A kind of 7. preparation method of alumina-coated noble metal catalyst according to claim 1, it is characterised in that：It is described The temperature of sealing pressing reaction in step 3 is 60-70 DEG C, pressure 2-5MPa.
- A kind of 8. preparation method of alumina-coated noble metal catalyst according to claim 1, it is characterised in that：It is described The concentration of nano-aluminum hydroxide in step 4 is 10-15mg/L, and platinum particles concentration is 2-8mg/L, and aerated reaction gas is nitrogen Or air, the flow velocity of the aerated reaction is 10-20mL/min, and aerated reaction temperature is 40-50 DEG C.
- A kind of 9. preparation method of alumina-coated noble metal catalyst according to claim 1, it is characterised in that：It is described The addition of crown ether in step 5 is 2-4 times of nano-aluminum hydroxide mole, mixing speed 1000-1500r/min.
- A kind of 10. preparation method of alumina-coated noble metal catalyst according to claim 1, it is characterised in that：Institute It is 200-400 DEG C to state the sintering temperature in step 6, and the grain diameter after milling is not more than 10 microns.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711049881.6A CN107649123A (en) | 2017-10-31 | 2017-10-31 | A kind of preparation method of alumina-coated noble metal catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711049881.6A CN107649123A (en) | 2017-10-31 | 2017-10-31 | A kind of preparation method of alumina-coated noble metal catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107649123A true CN107649123A (en) | 2018-02-02 |
Family
ID=61096247
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711049881.6A Pending CN107649123A (en) | 2017-10-31 | 2017-10-31 | A kind of preparation method of alumina-coated noble metal catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107649123A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807937A (en) * | 2018-07-09 | 2018-11-13 | 绍兴文理学院 | A kind of preparation method of the carbon silicon nanocomposite of lithium battery |
| CN109174086A (en) * | 2018-10-07 | 2019-01-11 | 吴亚良 | A kind of preparation method of high-performance noble metal catalyst |
| CN109301270A (en) * | 2018-11-06 | 2019-02-01 | 陕西瑞科新材料股份有限公司 | A kind of preparation method of high-performance ruthenium catalyst |
| CN111185155A (en) * | 2018-11-14 | 2020-05-22 | 中国科学院大连化学物理研究所 | Load-coated noble metal catalyst and preparation and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103606660A (en) * | 2013-11-06 | 2014-02-26 | 中国科学院化学研究所 | Alumina-coated granules, as well as preparation method and application thereof |
| CN105618033A (en) * | 2015-12-23 | 2016-06-01 | 上海大学 | Method for preparing mesoporous gamma-Al2O3 high-dispersion loaded palladium catalyst |
-
2017
- 2017-10-31 CN CN201711049881.6A patent/CN107649123A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103606660A (en) * | 2013-11-06 | 2014-02-26 | 中国科学院化学研究所 | Alumina-coated granules, as well as preparation method and application thereof |
| CN105618033A (en) * | 2015-12-23 | 2016-06-01 | 上海大学 | Method for preparing mesoporous gamma-Al2O3 high-dispersion loaded palladium catalyst |
Non-Patent Citations (2)
| Title |
|---|
| 林友文等: "《有机化学》", 31 July 2016 * |
| 赵桂良等: "含铂废催化剂综合利用技术进展", 《中外能源》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807937A (en) * | 2018-07-09 | 2018-11-13 | 绍兴文理学院 | A kind of preparation method of the carbon silicon nanocomposite of lithium battery |
| CN109174086A (en) * | 2018-10-07 | 2019-01-11 | 吴亚良 | A kind of preparation method of high-performance noble metal catalyst |
| CN109301270A (en) * | 2018-11-06 | 2019-02-01 | 陕西瑞科新材料股份有限公司 | A kind of preparation method of high-performance ruthenium catalyst |
| CN109301270B (en) * | 2018-11-06 | 2021-08-10 | 陕西瑞科新材料股份有限公司 | Preparation method of high-performance ruthenium catalyst |
| CN111185155A (en) * | 2018-11-14 | 2020-05-22 | 中国科学院大连化学物理研究所 | Load-coated noble metal catalyst and preparation and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107649123A (en) | A kind of preparation method of alumina-coated noble metal catalyst | |
| RU2675842C2 (en) | Alloy-comprising catalyst, method of preparation and uses | |
| CN101670286B (en) | Supported transition metal or transition metal alloy nanocluster catalyst and preparation method and application thereof | |
| EP3045227B1 (en) | Exhaust gas purification catalyst | |
| RU2730496C2 (en) | Rhodium-containing catalysts for treating automotive exhausts | |
| CN113477277B (en) | Composite material of metal-loaded covalent organic framework and preparation method and application thereof | |
| WO2016123534A1 (en) | Platinum group metal (pgm) catalysts for automotive emissions treatment | |
| CN102631917A (en) | Oxidation catalyst for purifying tail gas of diesel vehicle and preparation method for oxidation catalyst | |
| CN106999849A (en) | Use the triple effect catalytic converter of mixed catalytic particle | |
| CN109621918A (en) | A kind of amino functional porous material and its preparation method and application | |
| CN106824187A (en) | A kind of cerium zirconium compound oxide supports catalyst of platinum and its preparation method and application | |
| WO2008059858A1 (en) | Exhaust gas purifying catalyst | |
| CN109012665A (en) | A kind of double coating three-way catalysts and preparation method thereof | |
| CN104310979A (en) | Functional ceramic powder material as well as preparation method and application thereof | |
| JP2016013552A (en) | Catalyst for exhaust gas purification and production method thereof, and exhaust gas purification method | |
| JP2006181484A (en) | Catalyst, exhaust gas cleaning catalyst and method for preparing the catalyst | |
| CN109225210A (en) | A kind of low noble metal diesel vehicle oxidation catalyst preparation method and its catalyst of preparation | |
| CN1260242C (en) | Method for extracting DNA by using magnetic nano composite material and its kit | |
| CN110152721A (en) | The preparation method of wall-flow particulate trap catalyst | |
| CN101700497B (en) | Ternary catalyst for metal honeycomb carrier of motorcycle and method for preparing same | |
| CN103316658B (en) | A kind of nanometer composite cerium zirconium solid solution and preparation method thereof | |
| CN111939928A (en) | Three-way catalyst for enhancing durability of tail gas purification and preparation method thereof | |
| CN104056637A (en) | Preparation method of catalyst for vehicle exhaust purification | |
| CN103831101B (en) | A kind of catalyst coat reducing POC regeneration temperature | |
| CN111957313A (en) | Three-way catalyst for gasoline vehicle and its prepn |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180202 |