CN101161342B - Method for preparing high activity loading type RhxAu-x/Y nanometer catalyst - Google Patents

Method for preparing high activity loading type RhxAu-x/Y nanometer catalyst Download PDF

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CN101161342B
CN101161342B CN2007101779747A CN200710177974A CN101161342B CN 101161342 B CN101161342 B CN 101161342B CN 2007101779747 A CN2007101779747 A CN 2007101779747A CN 200710177974 A CN200710177974 A CN 200710177974A CN 101161342 B CN101161342 B CN 101161342B
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catalyst
metal
storage tank
slurries
tubular reactor
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CN101161342A (en
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何洪
关晓
杨柳
戴洪兴
訾学红
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Beijing University of Technology
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Beijing University of Technology
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Abstract

The method for preparing the high-activity loading type RhxAu1-x/Y nano catalyst belongs to the preparing field of the nana catalyzing material. The application of the noble metal catalyst in the purification of the vehicle tail gas gets a large attention from the people all the time. But the price of the noble metals of Pt, Pd and Rh is high and the resource dries up increasingly, so the reducing to the noble metal usage of the three-way catalyst and manufacturing cost is the problem that needs to be settled currently. The invention uses the RhxAu1-x/Y(Y equals to the metallic oxide) nano catalyst prepared with the ultrasound-assisted dropping reaction method (UAMAR) to reactions of oxidizing the carbon monoxide and NO reducing action, etc. the nano catalyst has an excellent activity andcan be used to displace the noble metal Rh catalyst too reduce the cost of the three-way catalyst. The preparing method overcomes the disadvantages of common impregnation method to prepare the loading type metal catalyst, and the prepared nana metal catalyst has the advantages of epigranular particles of active component, narrow distribution of particle size and high catalyzing activity.

Description

High activity loading type Rh xAu 1-xThe preparation method of/Y nanocatalyst
Technical field
The present invention relates to support type Rh xAu 1-xThe preparation method of/(Y=metal oxide) nanocatalyst is specifically related to adopt a series of support type Rh of ultrasonic barrier diffusion method (UAMR) preparation xAu 1-xThe preparation method of/Y (Y=metal oxide) nanocatalyst belongs to the preparation field of nano catalytic material, and the catalyst of this method preparation can be used for purifying vehicle exhaust.
Background technology
The application of noble metal catalyst in purifying vehicle exhaust receives people's very big concern always.Vehicle exhaust mainly contains CO, HC and NO xDeng pollutant, how effectively purifying automobile tail gas has become one of focus of paying close attention in the current whole world.At present commercially available cleaning catalyst for tail gases of automobiles major part is to be active component with Pt, Pd and Rh, with La 2O 3And CeO 2Be auxiliary agent, with γ-Al 2O 3It is the second carrier loaded noble metal type catalyst to ceramic honeycomb.Precious metals pt, Pd and Rh cost an arm and a leg and resource exhaustion day by day, are present urgent problems so reduce the noble metal dosage and the manufacturing cost of three-way catalyst.In the past few decades, people have carried out a large amount of utilize base metal or rare earth metal and have replaced the exploration of noble metal in the three-way catalyst, but, the result shows that noble metal can not be replaced fully, can only utilize improvement catalyst preparation process and the optimization of C consumption with the noble metal of reduction catalyst.Recently, if we find that the Rh metallic on the support type Rh metallic catalyst is prepared into nano particle can improve this activity of such catalysts, the Au element is introduced in the support type Rh metallic catalyst, make Au and Rh form alloy or bimetal nano particle, can improve and keep under the condition that three-effect catalysis model reaction activity do not reduce, reduce the consumption of metal Rh significantly.This catalyst has very strong practicality, can be used for the preparation of auto-pollution emission control triple effect catalytic converter.
At present, the preparation method of traditional preparation support type alloy catalyst mainly contains infusion process, coprecipitation, sol-gal process, chemical reduction method etc.The active component of the loaded catalyst of traditional preparation method's preparation is skewness often, and metal dispersity is low, and content of metal is big, the production cost height.Utilization of the present invention utilizes ultrasonic barrier diffusion method (UAMR) to prepare Rh xAu 1-x/ Y (Y=metal oxide) nanocatalyst, its catalyst three-effect catalysis reactive activity is higher than the pure Rh metallic catalyst by immersion process for preparing.
Summary of the invention
The object of the present invention is to provide a kind of high activity loading type Rh xAu 1-xThe preparation method of/Y (Y is that carrier material is a metal oxide) nanocatalyst.This catalyst can be used for replacing noble metal Rh catalyst, to reduce the cost of three-way catalyst.The present invention utilizes the Rh of ultrasonic barrier diffusion method (UAMR) preparation xAu 1-x/ Y (Y=metal oxide) nanocatalyst is to the carbon monoxide oxidation, and reactions such as NO reduction have good active, can be used for the automobile exhaust pollution emission control.Its preparation method has overcome the shortcoming of conventional immersion process for preparing load type metal catalyst, the support type Rh of preparation xAu 1-x/ Y (Y=metal oxide) nanocatalyst has the particles of active components epigranular, narrow diameter distribution, the advantage that catalytic activity is high.
Preparation equipment has been applied for patent of invention, denomination of invention: a kind of preparation method of load-type nanometer metal catalyst and equipment, application number: 200710118756.6, preparation equipment is characterized in that: complete equipment comprises measuring pump 1, metal salt solution storage tank 2, tubular reactor 4, supersonic generator 5, infusion pump 8, product storage tank 9, hollow ceramic membranes pipe 10; (figure-1)
Built-in hollow ceramic membranes pipe 10 (at least 3) in the tubular reactor 4, hollow ceramic membranes pipe 10 are evenly distributed and be fixed on epoxy resin on the black box 6 at tubular reactor 4 two ends (figure-2, figure-3) on the circle in the center of circle at the central shaft with tubular reactor 4.
Tubular reactor 4 places in the supersonic generator 5, and hollow ceramic membranes pipe 10 inlet 3 by tubular reactor 4 one end cavitys 11 and tubular reactor 4 is connected with measuring pump 1, and measuring pump 1 is connected with metal salt solution storage tank 2;
Tubular reactor 4 outlet 7 links to each other with product storage tank 9 by pipeline, and the another one inlet 12 of tubular reactor 4 is connected (scheming-1) by the pipelines of infusion pump 8 with product storage tank 9.
Preparation method of the present invention is as follows:
(I) according to Rh xAu 1-x, x=0.4～1.0 preparing metal salting liquids adds carrier material and stirs into slurries, and transfers in the product storage tank 9, and wherein metal salt solution is the mixing salt solution of Rh salt and Au salt;
(II) preparation reductant solution, the reducing agent in the reductant solution is 1: 1～15: 1 with metal molar ratio in the above-mentioned metal salt solution, reductant solution is transferred in the metal salt solution storage tank 2 then;
(III) start infusion pump 8, flow velocity is 500-1000ml/min, the slurries that contain slaine and carrier material is injected into the tubular reactor 4 through infusion pump 8 from product storage tank 9, and is back in the product storage tank 9, start supersonic generator 5 then, tranmitting frequency is 40-120KHz;
(IV) start measuring pump 1, flow velocity is 0.1-10ml/min, reductant solution is entered in hollow ceramic membranes 10 pipelines in the tubular reactor 4, be diffused into by the micropore on the hollow ceramic membranes duct wall in the exocoel of tubular reactor 4, contact with the slurries that contain slaine and carrier material, metal ion is at the carrier surface absorbing and reducing, the slurries that obtain are through centrifugation, the precipitate with deionized water washing was dried 4 hours for 80 ℃, and 500 ℃ of calcinations obtained high activity loading type Rh in 3 hours in muffle furnace xAu 1-x/ Y nanocatalyst.
The catalyst that obtains carries out tem observation, and choose model reaction in vent gas treatment three validity responses (CO oxidation reaction, NO+CO reaction) and carry out the catalyst activity property testing, and compare with the Rh/Y catalyst activity of the equal content of metal of traditional immersion process for preparing.
The chemical molecular expression formula of RhAu alloy catalyst of the present invention is Rh xAu 1-x/ Y (Y=metal oxide), described a kind of support type alloy nano catalyst is characterized in that: Rh xAu 1-xThe x value can be 0.4～1.0 in/Y (Y=metal oxide) catalyst.
Support type Rh of the present invention xAu 1-xThe preparation raw material of/Y (Y=metal oxide) nanocatalyst is AuCl 3, HAuCl 4, Au (NO 3) 3, RhCl 3NH 2O, H 3RhCl 6, Rh 2O 3NH 2O, Rh (NO 3) 3NH 2O, Rh 2(CH 3CO 2) 3, Rh (NO 3) 3
Carrier material is high-ratio surface material, for example γ-Al commonly used 2O 3, SiO 2, TiO 2, ZrO 2Or Ce 1-yZr yO 2(y=0～1.0) etc.
Described reducing agent is N 2H 4, NaBH 4, ascorbic acid, oxalic acid, formaldehyde or ethanol.
The invention has the beneficial effects as follows:
The support type Rh that utilizes the present invention to prepare xAu 1-x/ Y (Y=metal oxide) nanocatalyst has that cost is low, metal dispersity is high, activated centre component even particle size distribution, the little and catalytic activity advantages of higher of particle diameter.
Description of drawings
Fig. 1 prepares support type Rh xAu 1-xThe apparatus system schematic diagram of/Y (Y=metal oxide) nanocatalyst;
Fig. 2 tubular reactor structural representation;
Fig. 3 tubular reactor inner ceramic film distribution map;
Fig. 4 Rh (0.50wt%)/γ-Al 2O 3The TEM figure of nanocatalyst;
Fig. 5 Rh 0.5Au 0.5(0.50wt%)/γ-Al 2O 3The TEM figure of nanocatalyst;
The Rh of Fig. 6 UAMR method preparation xAu 1-x(0.50wt%)/the Catalyst for CO oxidation activity figure of the equal content of metal of Y nanocatalyst (x=1,0.8,0.6,0.5,0.4) and immersion process for preparing;
The Rh of Fig. 7 UAMR method preparation xAu 1-x(0.50wt%)/Catalyst for CO+NO reactivity figure of the equal content of metal of Y nanocatalyst (x=1,0.8,0.5) and immersion process for preparing;
The specific embodiment
Embodiment 1:
With 0.05 gram radium chloride (RhCl 3) be dissolved in the 200ml deionized water, add 5 gram γ-Al then 2O 3, fully stirring is transferred in the storage tank 9 after forming slurries; With 0.5 gram sodium borohydride (NaBH 4) be dissolved in the 50ml deionized water and transfer in the storage tank 2.Start infusion pump 8, make RhCl 3And γ-Al 2O 3Mixed serum between storage tank 9 and tubular reactor 4, circulate, flow velocity is 600ml/min, starts supersonic generator 5, the frequency that supersonic generator is set is 80KHZ, bath temperature is 40 ℃, measuring pump 1 with the speed of 1.0ml/min with NaBH 4Solution is injected in the pipeline of the hollow ceramic membranes pipe 10 in the tubular reactor 4, NaBH 4Solution is diffused into by the micropore on the hollow ceramic membranes tube wall and contains RhCl 3And γ-Al 2O 3Mixed serum in, work as NaBH 4After all adding, solution closes measuring pump 1, supersonic generator 5, utilize infusion pump 8 that the slurries in the tubular reactor 4 are all imported in the storage tank 9, close infusion pump 8, slurries are separated with centrifuge, after the precipitate with deionized water washing that obtains 3 times, 80 ℃ of oven dry 4 hours, 500 ℃ of calcinations were 3 hours in muffle furnace, promptly obtain Rh 1Au 0(0.50wt%)/γ-Al 2O 3Carrier nanometer catalyst is at γ-Al 2O 3On the carrier, the little and narrow particle size distribution (Fig. 4) of metal Rh particle diameter.Its CO oxidation and NO reduction reaction activity all be far superior to the same metal content of immersion process for preparing catalyst (Fig. 6, Fig. 7).
Embodiment 2:
With 0.04 gram rhodium nitrate (Rh (NO 3) 3) and 0.016 gram gold chloride (HAuCl 4) be dissolved in the 200ml deionized water, add 5 gram TiO then 2, fully stirring is transferred in the storage tank 9 after forming slurries; With 0.2 gram sodium borohydride (NaBH 4) be dissolved in the 50ml deionized water and transfer in the storage tank 2.Start infusion pump 8, make Rh (NO 3) 3, HAuCl 4And TiO 2Mixed serum between storage tank 9 and tubular reactor 4, circulate, flow velocity is 800ml/min, starts supersonic generator 5, the frequency that supersonic generator is set is 60KHZ, bath temperature is 40 ℃, measuring pump 1 with the speed of 3.0ml/min with NaBH 4Solution is injected in the pipeline of the hollow ceramic membranes pipe 10 in the tubular reactor 4, NaBH 4Solution is diffused into by the micropore on the hollow ceramic membranes tube wall and contains Rh (NO 3) 3, HAuCl 4And TiO 2Mixed serum in, work as NaBH 4After all adding, solution closes measuring pump 1, supersonic generator 5, utilize infusion pump 8 that the slurries in the tubular reactor 4 are all imported in the storage tank 9, close infusion pump 8, slurries are separated with centrifuge, after the precipitate with deionized water washing that obtains 3 times, 80 ℃ of oven dry 4 hours, 500 ℃ of calcinations were 3 hours in muffle furnace, promptly obtain Rh 0.8Au 0.2(0.50wt%)/TiO 2Carrier nanometer catalyst is with Rh (0.5wt%)/γ-Al of immersion process for preparing 2O 3Catalyst is compared, the Rh of UAMR method preparation 0.8Au 0.2(0.5wt%)/TiO 2The CO oxidation of catalyst, the reactivity of CO+NO all be better than the former (Fig. 6, Fig. 7).
Embodiment 3:
With 0.031 gram chlorine rhodium acid (H 3RhCl 6) and 0.02 gram chlorauride (AuCl 3) be dissolved in the 200ml deionized water, add 5 gram SiO then 2, fully stirring is transferred in the storage tank 9 after forming slurries; With 0.5mlN 2H 4Be dissolved in the 50ml deionized water and transfer in the storage tank 2.Start infusion pump 8, make H 3RhCl 6, AuCl 3And TiO 2Mixed serum between storage tank 9 and tubular reactor 4, circulate, flow velocity is 1000ml/min, starts supersonic generator 5, the frequency that supersonic generator is set is 100KHZ, bath temperature is 40 ℃, measuring pump 1 with the speed of 0.1ml/min with N 2H 4Solution is injected in the pipeline of the hollow ceramic membranes pipe 10 in the tubular reactor 4, N 2H 4Solution is diffused into by the micropore on the hollow ceramic membranes tube wall and contains H 3RhCl 6, AuCl 3And SiO 2Mixed serum in, work as N 2H 4After all adding, solution closes measuring pump 1, supersonic generator 5, utilize infusion pump 8 that the slurries in the tubular reactor 4 are all imported in the storage tank 9, close infusion pump 8, slurries are separated with centrifuge, after the precipitate with deionized water washing that obtains 3 times, 80 ℃ of oven dry 4 hours, 500 ℃ of calcinations were 3 hours in muffle furnace, promptly obtain Rh 0.6Au 0.4(0.50wt%)/SiO 2Carrier nanometer catalyst is with Rh (0.5wt%)/γ-Al of immersion process for preparing 2O 3Catalyst is compared, the Rh of UAMR method preparation 0.6Au 0.4(0.5wt%)/SiO 2The CO oxidation activity of catalyst be better than the former (Fig. 6).
Embodiment 4:
With 0.025 gram rhodium oxide (Rh 2O 3H 2O) and 0.032 gram gold chloride (HAuCl 4) be dissolved in the 200ml deionized water, add 5 gram γ-Al then 2O 3, fully stirring is transferred in the storage tank 9 after forming slurries; 1 gram oxalic acid is dissolved in the 50ml deionized water and transfers in the storage tank 2.Start infusion pump 8, make Rh 2O 3H 2O, HAuCl 4And γ-Al 2O 3Mixed serum between storage tank 9 and tubular reactor 4, circulate, flow velocity is 500ml/min, start supersonic generator 5, the frequency that supersonic generator is set is 40KHZ, bath temperature is 60 ℃, measuring pump 1 is injected into oxalic acid solution in the pipeline of the hollow ceramic membranes pipe 10 in the tubular reactor 4 with the speed of 10ml/min, and oxalic acid solution is diffused into by the micropore on the hollow ceramic membranes tube wall and contains Rh 2O 3H 2O, HAuCl 4And γ-Al 2O 3Mixed serum in, after all adding, oxalic acid solution closes measuring pump 1, supersonic generator 5, utilize infusion pump 8 that the slurries in the tubular reactor 4 are all imported in the storage tank 5, close infusion pump 8, slurries are separated with centrifuge, after the precipitate with deionized water that obtains is washed 3 times, 80 ℃ of oven dry 4 hours, 500 ℃ of calcinations are 3 hours in muffle furnace, promptly obtain Rh 0.5Au 0.5(0.50wt%)/γ-Al 2O 3Carrier nanometer catalyst is at γ-Al 2O 3On the carrier, the alloy particle particle diameter is 4-6nm and narrow particle size distribution (Fig. 5).Rh (0.5wt%)/γ-Al with immersion process for preparing 2O 3Catalyst is compared, the Rh of UAMR method preparation 0.5Au 0.5(0.5wt%)/γ-Al 2O 3The CO oxidation activity of catalyst be better than the former (Fig. 6), the reactivity of CO+NO is similar to the former
(Fig. 7).
Embodiment 5:
With 0.013 gram radium chloride (RhCl 3) and 0.035 gram nitric acid gold (Au (NO 3) 3) be dissolved in the 200ml deionized water, add 5 gram ZrO then 2, fully stirring is transferred in the storage tank 9 after forming slurries; Be dissolved in ascorbic acid in the 50ml deionized water and transfer in the storage tank 2.Start infusion pump 8, make RhCl 3, Au (NO 3) 3And ZrO 2Mixed serum between storage tank 9 and tubular reactor 4, circulate, flow velocity is 700ml/min, start supersonic generator 5, the frequency that supersonic generator is set is 120KHZ, bath temperature is 40 ℃, measuring pump 1 is injected into ascorbic acid solution in the pipeline of the hollow ceramic membranes pipe 10 in the tubular reactor 4 with the speed of 7.0ml/min, and ascorbic acid solution is diffused into by the micropore on the hollow ceramic membranes tube wall and contains RhCl 3, Au (NO 3) 3And ZrO 2Mixed serum in, after all adding, ascorbic acid solution closes measuring pump 1, supersonic generator 5, utilize infusion pump 8 that the slurries in the tubular reactor 4 are all imported in the storage tank 9, close infusion pump 8, slurries are separated with centrifuge, after the precipitate with deionized water that obtains is washed 3 times, 80 ℃ of oven dry 4 hours, 500 ℃ of calcinations are 3 hours in muffle furnace, promptly obtain Rh 0.4Au 0.6(0.50wt%)/ZrO 2Carrier nanometer catalyst, the Rh of UAMR method preparation 0.4Au 0.6(0.5wt%)/ZrO 2The CO oxidation activity of catalyst is better than Rh (0.5wt%)/γ-Al of immersion process for preparing 2O 3Catalyst (Fig. 6).

Claims (1)

1. high activity loading type Rh xAu 1-xThe preparation method of/Y nanocatalyst, wherein Y is a metal oxide as carrier material, it is characterized in that, preparation process is as follows:
(I) according to Rh xAu 1-x, x=0.4～1.0 preparing metal salting liquids adds carrier material and stirs into slurries, and transfers in the product storage tank (9), and wherein metal salt solution is the mixing salt solution of Rh salt and Au salt;
(II) preparation reductant solution, the reducing agent in the reductant solution is 1: 1～15: 1 with metal molar ratio in the above-mentioned metal salt solution, then reductant solution is transferred in the metal salt solution storage tank (2);
(III) start infusion pump (8), flow velocity is 500-1000ml/min, the slurries that contain slaine and carrier material are injected into the tubular reactor (4) through infusion pump (8) from product storage tank (9), and be back in the product storage tank (9), start supersonic generator (5) then, tranmitting frequency is 40-120KHz;
(IV) start measuring pump (1), flow velocity is 0.1-10ml/min, reductant solution is entered in interior hollow ceramic membranes (10) pipeline of tubular reactor (4), be diffused into by the micropore on the hollow ceramic membranes duct wall in the exocoel of tubular reactor (4), contact with the slurries that contain slaine and carrier material, metal ion is at the carrier surface absorbing and reducing, the slurries that obtain are through centrifugation, the precipitate with deionized water washing, dried 4 hours for 80 ℃, 500 ℃ of calcinations obtained high activity loading type Rh in 3 hours in muffle furnace xAu 1-x/ Y nanocatalyst,
Wherein the reducing agent of step (II) is N 2H 4, NaBH 4, ascorbic acid, oxalic acid, formaldehyde or ethanol,
Wherein the carrier material of step (I) is γ-Al 2O 3, SiO 2, TiO 2, ZrO 2Or Ce 1-yZr yO 2, y=0～1.0.
CN2007101779747A 2007-11-23 2007-11-23 Method for preparing high activity loading type RhxAu-x/Y nanometer catalyst Expired - Fee Related CN101161342B (en)

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GB201110850D0 (en) * 2011-03-04 2011-08-10 Johnson Matthey Plc Catalyst and mehtod of preparation
US9115621B2 (en) 2011-03-04 2015-08-25 Toyota Jidosha Kabushiki Kaisha Metal particles, exhaust gas purifying catalyst comprising metal particles, and methods for producing them
US9114384B2 (en) 2011-08-23 2015-08-25 Toyota Jidosha Kabushiki Kaisha Exhaust gas purification catalyst and method for producing it
CN103816898B (en) * 2014-03-11 2016-07-06 北京工业大学 A kind of have the AuRh nanometer particle load type catalyst of nucleocapsid structure, preparation method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1251323A (en) * 1999-09-17 2000-04-26 厦门大学 Preparation for load type gold catalyst by bacterial reduction method
US6558575B2 (en) * 2001-02-07 2003-05-06 Agfa-Gevaert Perparation of improved ZnS:Mn phosphors
CN1907556A (en) * 2006-07-19 2007-02-07 北京工业大学 Method and apparatus for preparing inorganic oxidate or metallic nano-particle

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1251323A (en) * 1999-09-17 2000-04-26 厦门大学 Preparation for load type gold catalyst by bacterial reduction method
US6558575B2 (en) * 2001-02-07 2003-05-06 Agfa-Gevaert Perparation of improved ZnS:Mn phosphors
CN1907556A (en) * 2006-07-19 2007-02-07 北京工业大学 Method and apparatus for preparing inorganic oxidate or metallic nano-particle

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