CN101856612B - Preparation method of nanometer noble metal catalyst - Google Patents
Preparation method of nanometer noble metal catalyst Download PDFInfo
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- CN101856612B CN101856612B CN 201010189525 CN201010189525A CN101856612B CN 101856612 B CN101856612 B CN 101856612B CN 201010189525 CN201010189525 CN 201010189525 CN 201010189525 A CN201010189525 A CN 201010189525A CN 101856612 B CN101856612 B CN 101856612B
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Abstract
The invention discloses a preparation method of a nanometer noble metal catalyst, which comprises the following steps: regulating the pH value of noble metal salt solution to 2-10; adding deionized water to enable the total volume of the solution to be equal to the pore volume of a carrier; adding the carrier and dipping; adding ammonia water the pH of which is equal to 10-11 or deionized water for aging; filtering, washing and drying to obtain a catalyst precursor; and heating the catalyst precursor in hydrogen or air to 100-300 DEG C at the speed of 2-15 DEG C/min, and then preserving the temperature of 100-300 DEG C for 0.5-3 hours to obtain the nanometer noble metal catalyst. The preparation method of the nanometer noble metal catalyst of the invention is simple, does not need to strictly control the pH value of dipping solution, and can prepare the loaded nanometer noble metal catalyst with high catalytic activity, high response stability and storage stability in a wider pH range.
Description
Technical field
The present invention relates to the preparing technical field of nanocatalyst, particularly a kind of method for preparing high activity, high-stability nano noble metal catalyst under wider pH value condition.
Background technology
Loaded noble metal catalyst is the novel environmental friendly catalysis material of a class, and many reactions such as CO low-temperature oxidation are had good catalytic performance, at indoor and purifications industrial gasses, closed CO
2The closed environments such as laser instrument, submarine, spacecraft, safe breathing mask, the CO gas sensor, the aspects such as hydrogen fuel cell are or be about to be widely used.
Al
2O
3Stable in properties is easy to moulding, is industrial catalyst carrier commonly used, with Al
2O
3And composite oxides MO
x/ Al
2O
3For the nano-noble metal catalyst of carrier demonstrates good catalytic performance in many reactions such as CO oxidation.At present, prepare the traditional deposition-precipitation method of the many employings of method of such catalyst, although this method has many advantages, need heating in preparation process, especially need strictly to control the pH value of reaction solution, just can make the higher loaded catalyst of catalytic activity.As document Donghui Wang, Zhengping Hao, Daiyun Cheng, Xicheng Shi, Chun Hu, J.Mol.Catal.A., 200,229 (2003) and Shixue Qi, Xuhua Zou, Xufeng Xu, Lidun An, Shuben Li, Chin.J.Mol.Catal., 16,139 (2002) etc. all adopt deposition-precipitation method, be respectively under 8.0～8.5 and 6.5～7.0 conditions in the pH value, made respectively the higher Au/TiO of initial catalytic activity
2And Au/FeO
x/ Al
2O
3Catalyst.In addition, document S.J.Lee, A.Gavriilidis, J.Catal.206,305 (2002) and Zhanghuai Suo, Yonggen Weng, Mingshan Jin, Aihua Lu, Jinguang Xu, LidunAn, Chin.J.Catal., a kind of anion infusion processes of employing such as 26,1022 (2005) have prepared Au/Al
2O
3Catalyst, this method need not heat in preparation process, and within the specific limits, the pH value of dipping solution is higher, and the initial activity that makes catalyst CO oxidation is higher.And the problems such as the less stable that such catalyst shows in the CO oxidation reaction, the rear easily inactivation of storage make it fail so far to be widely used under actual conditions.Therefore, be badly in need of at present a kind of pH value that does not need strictly to control dipping solution, can make the method for the nano-noble metal catalyst of high catalytic activity, especially high reaction stability and storage stability under wider pH value condition.
Summary of the invention
The purpose of this invention is to provide that a kind of more traditional deposition-precipitation method is simple and effective, the suitable method for preparing high activity, high-stability nano noble metal catalyst under wider pH value condition.
The method for preparing nano-noble metal catalyst provided by the present invention comprises the steps:
With precious metal salt solution the pH value be adjusted to 2～10, add deionized water to make the cumulative volume of solution equal the pore volume of carrier, add carrier, the dipping;
The ammoniacal liquor or the deionized water ageing that add pH=10～11 then after filtration, washing, drying, obtain catalyst precarsor;
Described catalyst precarsor speed with 2～15 ℃/minute in hydrogen or air is warming up to 100～300 ℃, keeps 0.5～3 hour at 100～300 ℃, obtains nano-noble metal catalyst.
The method for preparing nano-noble metal catalyst of the present invention, wherein: the molar concentration of described precious metal salt solution is 0.01～0.15mol/L.
The method for preparing nano-noble metal catalyst of the present invention, wherein: described noble metal be in Au, Pt, Pd any one or appoint several.
The method for preparing nano-noble metal catalyst of the present invention, wherein: described carrier is Al
2O
3Or MO
x/ Al
2O
3Described M is any one or a few in Fe, Co, Ni, Cu, Zn, Mg, Mn, Ce, Li, Rb, La, Ti, Cr.
The method for preparing nano-noble metal catalyst of the present invention, wherein: described MO
x/ Al
2O
3The load capacity of middle MOx is 0.05～10% of gross weight.
The method for preparing nano-noble metal catalyst of the present invention, wherein: the specific area of described carrier is 50～300m
2/ g, pore volume are 1.5～4.0ml/g.
The method for preparing nano-noble metal catalyst of the present invention, wherein: described precious metal salt is HAuCl
4, H
2PtCl
6Or (NH
4)
2PdCl
4
The method for preparing nano-noble metal catalyst of the present invention, wherein: the amount of described ammoniacal liquor or deionized water is the described carrier of the every gram of 10～20ml.
The method for preparing nano-noble metal catalyst of the present invention, wherein: carrier MO
x/ Al
2O
3The preparation of employing infusion process, process is as follows: with the salting liquid of metal M carrier A l
2O
3Dipping, standing 1～3h, drying, roasting and make.
The method for preparing nano-noble metal catalyst of the present invention does not need strictly to control the pH value of dipping solution, can make the loaded nano noble metal catalyst of high catalytic activity, high reaction stability and storage stability in wider pH scope.
The method for preparing nano-noble metal catalyst of the present invention is easy, the Al of preparation
2O
3And composite oxides MO
x/ Al
2O
3The nano-noble metal catalyst particle of load is in the scope of 2～5nm.
The specific embodiment
Embodiment 1:
With the KOH solution of the 0.1mol/L HAuCl with 0.01mol/L
4The pH value of solution is adjusted to 2, then adds deionized water, makes the cumulative volume of solution equal the pore volume of carrier; With carrier A l
2O
3Join in mentioned solution and flooded 1 hour, carrier A l
2O
3Pore volume be 1.5ml/g, specific area is 50m
2/ g; Add the ammoniacal liquor of pH=11 to soak 24h as maturing agent, the amount of ammoniacal liquor is the every gram carrier of 20ml again; Then after filtration, washing, 60 ℃ of dryings 18 hours obtain the precursor of catalyst, precursor is placed in tube furnace passes into hydrogen, are warming up to 200 ℃ with the speed of 2 ℃/minute, keep 3 hours, obtain the nano catalyst of high dispersive.
Nanometer Au/Al
2O
3In catalyst, Au accounts for 1.40% of gross weight, and the pay(useful) load rate of Au is 93%, and the size of gold grain is at 2～5nm.
Consist of in feed gas volume: CO:1%; O
2: 12%; N
2: 87%, the gas volume air speed is 15000h
-1Situation under, CO is converted into CO fully
2The permission minimum response temperature (being called " minimum full conversion temperature ", as follows) of (remaining CO is lower than Qi Xiang Se Spectrum detectable limit 0.005%) is-24 ℃.
With the unstripped gas of above-mentioned composition with 4.5 * 10
4h
-1Air speed, under 30 ℃ continuously by the fixed bed reactors successive reaction 18h of 0.2g catalyst is housed, the CO infrared analyzer detects CO transit dose≤0.02% online.
The stable storing property testing: catalyst takes out after 90 days through sealed storage, the reaction repeated stability test, and under the same test condition, the time that catalyst can make CO detect transit dose≤0.02% still is 18h.
Embodiment 2:
With the KOH solution of the 0.5mol/L H with 0.15mol/L
2PtCl
6The pH value of solution is adjusted to 5, then adds deionized water, makes the cumulative volume of solution equal the pore volume of carrier; With carrier A l
2O
3Join in mentioned solution and flooded 2 hours, carrier A l
2O
3Pore volume be 4.0ml/g, specific area is 300m
2/ g; Add the weak aqua ammonia of pH=11 to soak 24h as maturing agent, the amount of ammoniacal liquor is the every gram carrier of 15ml again; Then after filtration, washing, 60 ℃ of dryings 18 hours obtain the precursor of catalyst, precursor is placed in tube furnace passes into hydrogen, are warming up to 300 ℃ with the speed of 5 ℃/minute, keep 1 hour, obtain the NanoPt catalyst of high dispersive.
Nanometer Pt/Al
2O
3In catalyst, Pt accounts for 1.36% of gross weight, and the pay(useful) load rate of Pt is that the size of 91%, Pt particle is mainly at 2～5nm.
Initial activity test: consist of at unstripped gas: CO:1%; O
2: 12%; N
2: 87%, the gas volume air speed is 15000h
-1Situation under, CO is converted into CO fully
2Minimum full conversion temperature be-27 ℃.
The stable reaction property testing: with the unstripped gas of above-mentioned composition with 4.5 * 10
4h
-1Air speed, under 30 ℃ continuously by the fixed bed reactors successive reaction 55h of 0.2g catalyst is housed, the CO infrared analyzer detects CO transit dose≤0.02% online.
The stable storing property testing: catalyst takes out after 90 days through sealed storage, the reaction repeated stability test, and under the same test condition, the time that catalyst can make CO detect transit dose≤0.02% still is 55h.
Embodiment 3:
With the KOH solution of the 1.5mol/L (NH with 0.02mol/L
4)
2PdCl
4The pH value of solution is adjusted to 8, then adds deionized water, makes the cumulative volume of solution equal the pore volume of carrier; With carrier A l
2O
3Join in mentioned solution and flooded 3 hours, carrier A l
2O
3Pore volume be 3.0ml/g, specific area is 200m
2/ g; Add the weak aqua ammonia of pH=10 to soak 15h as maturing agent, the amount of ammoniacal liquor is the every gram carrier of 15ml again; Then after filtration, washing, 60 ℃ of dryings 18 hours obtain the precursor of catalyst, precursor is placed in tube furnace passes into hydrogen, are warming up to 300 ℃ with the speed of 4 ℃/minute, keep 2 hours, obtain the nano Pd catalyst of high dispersive.
Nanometer Pd/Al
2O
3In catalyst, Pd accounts for 1.35% of gross weight, and the pay(useful) load rate of Pd is that the size of 90%, Pd particle is mainly at 2～5nm.
Consist of at unstripped gas: CO:1%; O
2: 12%; N
2: 87%, the gas volume air speed is 15000h
-1Situation under, CO is converted into CO fully
2Minimum full conversion temperature be-26 ℃.
With the unstripped gas of above-mentioned composition with 4.5 * 10
4h
-1Air speed, under 30 ℃ continuously by the fixed bed reactors successive reaction 50h of 0.2g catalyst is housed, the CO infrared analyzer detects CO transit dose≤0.02% online.
The stable storing property testing: catalyst takes out after 90 days through sealed storage, the reaction repeated stability test, and under the same test condition, the time that catalyst can make CO detect transit dose≤0.02% still is 50h.
Embodiment 4:
With the KOH solution of the 0.5mol/L HAuCl with 0.05mol/L
4The pH value of solution is adjusted to 10, then adds deionized water, makes the cumulative volume of solution equal the pore volume of carrier; With carrier FeOx/Al
2O
3(load capacity of FeOx be gross weight 10%) joined in mentioned solution dipping 5 hours, carrier FeOx/Al
2O
3Pore volume be 2.0ml/g, specific area is 150m
2/ g; The weak aqua ammonia of pH=10 soaks 12h as maturing agent, and the amount of ammoniacal liquor is the every gram carrier of 10ml; Then after filtration, washing, 60 ℃ of dryings 18 hours obtain the precursor of catalyst, precursor is placed in tube furnace passes into air, are warming up to 250 ℃ with the speed of 3 ℃/minute, keep 2 hours, obtain the nano-Au catalyst of high dispersive.
Nanometer Au/FeOx/Al
2O
3In catalyst, Au accounts for 1.35% of gross weight, and the pay(useful) load rate of Au is 90%, and the size of gold grain is mainly at 2～5nm.
Consist of at unstripped gas: CO:1%; O
2: 12%; N
2: 87%, the gas volume air speed is 15000h
-1Situation under, CO is converted into CO fully
2Minimum full conversion temperature be-28 ℃.
With the unstripped gas of above-mentioned composition with 4.5 * 10
4h
-1Air speed, under 30 ℃ continuously by the fixed bed reactors successive reaction 52h of 0.2g catalyst is housed, the CO infrared analyzer detects CO transit dose≤0.02% online.
The stable storing property testing: catalyst takes out after 90 days through sealed storage, the reaction repeated stability test, and under the same test condition, the time that catalyst can make CO detect transit dose≤0.02% still is 52h.
Embodiment 5:
With the KOH solution of the 0.5mol/L HAuCl with 0.08mol/L
4The pH value of solution is adjusted to 7, then adds deionized water, makes the cumulative volume of solution equal the pore volume of carrier; With support C oOx/Al
2O
3(load capacity of CoOx be gross weight 1%) joined in mentioned solution dipping 5 hours, support C oOx/Al
2O
3Pore volume be 3.0ml/g, specific area is 200m
2/ g; The weak aqua ammonia of pH=11 soaks 10h as maturing agent, and the amount of ammoniacal liquor is the every gram carrier of 10ml; Then after filtration, washing, 60 ℃ of dryings 18 hours obtain the precursor of catalyst, precursor is placed in tube furnace passes into air, are warming up to 250 ℃ with the speed of 4 ℃/minute, keep 2.5 hours, obtain the nano catalyst of high dispersive.
Nanometer Au/CoOx/Al
2O
3In catalyst, Au accounts for 1.36% of gross weight, and the pay(useful) load rate of Au is 91%, and the size of gold grain is mainly at 2～5nm.
Consist of at unstripped gas: CO:1%; O
2: 12%; N
2: 87%, the gas volume air speed is 15000h
-1Situation under, CO is converted into CO fully
2Minimum full conversion temperature be-28 ℃.
With the unstripped gas of above-mentioned composition with 4.5 * 10
4h
-1Air speed, under 30 ℃ continuously by the fixed bed reactors successive reaction 55h of 0.2g catalyst is housed, the CO infrared analyzer detects CO transit dose≤0.02% online.
The stable storing property testing: catalyst takes out after 90 days through sealed storage, the reaction repeated stability test, and under the same test condition, the time that catalyst can make CO detect transit dose≤0.02% still is 55h.
Embodiment 6:
With the KOH solution of the 0.5mol/L HAuCl with 0.10mol/L
4The pH value of solution is adjusted to 8, then adds deionized water, makes the cumulative volume of solution equal the pore volume of carrier; With carrier NiOx/Al
2O
3(load capacity of NiOx be gross weight 2.5%) joined in mentioned solution dipping 8 hours, carrier NiOx/Al
2O
3Pore volume be 3.0ml/g, specific area is 200m
2/ g; The weak aqua ammonia of pH=11 soaks 10h as maturing agent, and the amount of ammoniacal liquor is the every gram carrier of 15ml; Then after filtration, washing, 60 ℃ of dryings 18 hours obtain the precursor of catalyst, precursor is placed in tube furnace passes into air, are warming up to 250 ℃ with the speed of 4 ℃/minute, keep 2.5 hours, obtain the nano catalyst of high dispersive.
Nanometer Au/NiOx/Al
2O
3In catalyst, Au accounts for 1.38% of gross weight, and the pay(useful) load rate of Au is 92%, and the size of gold grain is mainly at 2～5nm.
Consist of at unstripped gas: CO:1%; O
2: 12%; N
2: 87%, the gas volume air speed is 15000h
-1Situation under, CO is converted into CO fully
2Minimum full conversion temperature be-26 ℃.
With the unstripped gas of above-mentioned composition with 4.5 * 10
4h
-1Air speed, under 30 ℃ continuously by the fixed bed reactors successive reaction 48h of 0.2g catalyst is housed, the CO infrared analyzer detects CO transit dose≤0.02% online.
The stable storing property testing: catalyst takes out after 90 days through sealed storage, the reaction repeated stability test, and under the same test condition, the time that catalyst can make CO detect transit dose≤0.02% still is 48h.
Embodiment 7:
With the KOH solution of the 0.5mol/L HAuCl with 0.20mol/L
4And 0.20mol/L (NH
4)
2PdCl
4The pH value of mixed solution be adjusted to 8, then add deionized water, make the cumulative volume of solution equal the pore volume of carrier; With carrier A l
2O
3Join in mentioned solution and flooded 8 hours, carrier A l
2O
3Pore volume be 3.0ml/g, specific area is 200m
2/ g; The weak aqua ammonia of pH=11 soaks 10h as maturing agent, and the amount of ammoniacal liquor is the every gram carrier of 15ml; Then after filtration, washing, 60 ℃ of dryings 18 hours obtain the precursor of catalyst, precursor is placed in tube furnace passes into hydrogen, are warming up to 300 ℃ with the speed of 5 ℃/minute, keep 2 hours, obtain nanometer Au and the Pd catalyst of high dispersive.
Nanometer Au+Pd/Al
2O
3In catalyst, Au and Pd account for 1.35% of gross weight, and the pay(useful) load rate of Au+Pd is that the size of 90%, Au and Pd particle is mainly at 2～5nm.
Consist of at unstripped gas: CO:1%; O
2: 12%; N
2: 87%, the gas volume air speed is 15000h
-1Situation under, CO is converted into CO fully
2Minimum full conversion temperature be-27 ℃.
With the unstripped gas of above-mentioned composition with 4.5 * 10
4h
-1Air speed, under 30 ℃ continuously by the fixed bed reactors successive reaction 55h of 0.2g catalyst is housed, the CO infrared analyzer detects CO transit dose≤0.02% online.
The stable storing property testing: catalyst takes out after 90 days through sealed storage, the reaction repeated stability test, and under the same test condition, the time that catalyst can make CO detect transit dose≤0.02% still is 55h.
Embodiment 8:
With the KOH solution of the 1mol/L HAuCl with 0.5mol/L
4The pH value of solution is adjusted to 9, then adds deionized water, makes the cumulative volume of solution equal the pore volume of carrier; With carrier A l
2O
3Join in mentioned solution and flooded 2 hours, carrier A l
2O
3Pore volume be 1.5ml/g, specific area is 50m
2/ g; Add deionized water to soak 24h as maturing agent, the amount of deionized water is the every gram carrier of 20ml again; Then after filtration, washing, 60 ℃ of dryings 18 hours obtain the precursor of catalyst, precursor is placed in tube furnace passes into hydrogen, are warming up to 300 ℃ with the speed of 2 ℃/minute, keep 1.5 hours, obtain the nano catalyst of high dispersive.
Nanometer Au/Al
2O
3In catalyst, Au accounts for 1.38% of gross weight, and the pay(useful) load rate of Au is 92%, and the size of gold grain is at 2～5nm.
Consist of at unstripped gas: CO:1%; O
2: 12%; N
2: 87%, the gas volume air speed is 15000h
-1Situation under, CO is converted into CO fully
2Minimum full conversion temperature be-28 ℃.
With the unstripped gas of above-mentioned composition with 4.5 * 10
4h
-1Air speed, under 30 ℃ continuously by the fixed bed reactors successive reaction 56h of 0.2g catalyst is housed, the CO infrared analyzer detects CO transit dose≤0.02% online.
The stable storing property testing: catalyst takes out after 90 days through sealed storage, the reaction repeated stability test, and under the same test condition, the time that catalyst can make CO detect transit dose≤0.02% still is 56h.
Above embodiment is described the preferred embodiment of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineers and technicians in this area make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (5)
1. the preparation method of a nano-noble metal catalyst, is characterized in that: comprise the steps:
The pH value of precious metal salt solution is adjusted to 2 ~ 7, adds deionized water to make the cumulative volume of solution equal the pore volume of carrier, add carrier, dipping; Described noble metal is any one or a few in Au, Pt, Pd, and the molar concentration of precious metal salt solution is 0.01 ~ 0.15mol/L; Described carrier is Al
2O
3Or MO
x/ Al
2O
3Described M is any one or a few in Fe, Co, Ni, Cu, Zn, Mg, Mn, Ce, Li, Rb, La, Ti, Cr;
The ammoniacal liquor or the deionized water ageing that add pH=10 ~ 11 then after filtration, washing, drying, obtain catalyst precarsor;
Described catalyst precarsor speed with 2 ~ 15 ℃/minute in hydrogen or air is warming up to 100～300 ℃, keeps 0.5 ~ 3 hour at 100～300 ℃, obtains nano-noble metal catalyst.
2. method according to claim 1, is characterized in that: described MO
x/ Al
2O
3Middle MO
xLoad capacity be 0.05 ~ 10% of gross weight.
3. method according to claim 2, it is characterized in that: the specific area of described carrier is 50 ~ 300m
2/ g, pore volume are 1.5 ~ 4.0ml/g.
4. method according to claim 1, it is characterized in that: described precious metal salt is HAuCl
4, H
2PtCl
6Or (NH
4)
2PdCl
4
5. method according to claim 1, it is characterized in that: the amount of described ammoniacal liquor or deionized water is the described carrier of the every gram of 10 ~ 20ml.
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| CN101972650A (en) * | 2010-10-22 | 2011-02-16 | 烟台大学 | Nanometer noble metal catalyst with high reaction stability and preparation method thereof |
| CN103071511B (en) * | 2013-01-23 | 2014-08-06 | 岚晟新材料科技（上海）有限公司 | Preparation method of CO room-temperature catalyst with super-high activity and moisture resistance |
| CN103623842B (en) * | 2013-12-17 | 2015-04-08 | 烟台大学 | Granular supported nano gold catalyst for closed CO2 laser device |
| CN106334555A (en) * | 2016-11-15 | 2017-01-18 | 烟台大学 | High-activity and high-stability supported nanometer gold catalyst, preparation and application method |
| CN107715872A (en) * | 2017-10-31 | 2018-02-23 | 中国石油大学(华东) | A kind of super high-specific-surface mesoporous alumina load gold nano catalyst（Au/γ‑Al2O3）Synthetic method |
| CN114984940B (en) * | 2022-06-02 | 2023-06-06 | 宁波方太厨具有限公司 | PGM-Au alloy and preparation method and application thereof |
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| CN1736608A (en) * | 2005-07-06 | 2006-02-22 | 北京化工大学 | One-step method for preparing compound oxide supported nano noble metal catalyst |
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| CN1736608A (en) * | 2005-07-06 | 2006-02-22 | 北京化工大学 | One-step method for preparing compound oxide supported nano noble metal catalyst |
Non-Patent Citations (6)
| Title |
|---|
| CO低温氧化Au/Al2O3催化剂的失活及温度性;邹旭华等;《催化学报》;20060228;第27卷(第2期);第162页的"1、实验部分" * |
| Donghui Wang et al.,.Influence of pretreatment conditions on low-temperature CO oxidation over Au/MOx/Al2O3 catalysts.《Journal of Molecular Catalysis A:Chemical》.2003,(第200期),全文. |
| Donghui Wang et al.,.Influence of the calcination temperature on the Au/FeOx/Al2O3 catalysts.《J Chem Technol Biotechnol》.2006,(第81期),全文. |
| Influence of pretreatment conditions on low-temperature CO oxidation over Au/MOx/Al2O3 catalysts;Donghui Wang et al.,;《Journal of Molecular Catalysis A:Chemical》;20031231(第200期);全文 * |
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