CN105727943A - Method for synthesizing nano three-way catalyst - Google Patents
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Abstract
The invention provides a method for synthesizing a nano three-way catalyst and belongs to the technical field of a catalyst preparation process. The method takes a metal organic salt and a commercial carrier as raw materials and comprises the following steps: reacting in a solvent at 60-300 DEG C for 1-720 minutes; and controlling experimental parameters including a mol ratio of reactants, the concentration of the reactants, a reducing agent, a reaction temperature and the like to form the nano three-way catalyst which is formed in series and has controllable structure, shape and size. The method provided by the invention has the advantages that the raw materials are cheap and easy to obtain, time for a reaction is short, the solvent can be repeatedly utilized, the equipment is simple, and the method is easy to realize and control, has good process repeatability and stable product quality, is safe and reliable to operate, and is suitable for industrial large-scale production.
Description
Technical field
The present invention relates to the synthetic method of a kind of nanometer of three-way catalyst powder body, belong to catalyst preparation process technical field.
Background technology
In recent years, along with economic development, living standards of the people promote, and resident's automobile pollution continues to raise, and the impact of environment is become increasingly conspicuous by tail gas pollution of motor-driven vehicle.Three-way catalyst can effectively remove the hazardous air pollutants such as the Hydrocarbon in motor-vehicle tail-gas, nitrogen oxides and carbon monoxide, has been widely used, and multinational government compulsive requirement motor vehicles installation load must have the exhaust gas processing device of three-way catalyst.Prominent due to environmental problem, the requirement for three-way catalyst performance also improves day by day.
At present, many employings that improve of three-way catalyst are adulterated the method for promoter of other compositions in the carrier, seldom relate to the preparation of precious metal partial.And the preparation of noble metal catalyst part generally uses infusion process (AppliedCatalysisB:Environmental, 163 volumes, 499-509 page, 2015), the noble metal size in catalyst is often relatively big, and using rate of metal is low, and technology controlling and process is more difficult, catalytic efficiency is difficult to promote.
In recent years, nano science high speed development, occur in that a lot of method synthesizing noble metal nano particles.Wang etc. (Nature, 437 volumes, 121-124 page, 2005) develop a kind of universal method to synthesize noble metal nano particles, the method, with oleic acid, second alcohol and water for solvent, synthesizes noble metal nano particles in hydrothermal system.But needing relatively low solution concentration, in water heating kettle, pressure is relatively big, temperature required higher, thus limits throughput, there is again certain safety problem after amplification；(the JournaloftheAmericanChemicalSociety such as Mazumder, 131 volumes, 4588-4589 page, 2009) develop with oleyl amine for solvent and surfactant, precious metal salt is the method for predecessor, but solvent for use oleyl amine is expensive, and solvent for use is not readily separated, follow-up also need to load on carrier, loading process also easily produces precious metal losses, cause complex process, relatively costly, it is difficult to amplify and produce.Hydro-thermal, oleyl amine, enuatrol etc., but yield poorly, need back loading to cause damage and process complications limits its industrial applications, in order to effectively control tail gas pollution, a kind of catalyst particle size of development homogeneous controlled, technology difficulty is low, being easy to industrialized production, the method for preparing catalyst that precious metal atom utilization rate is high and catalytic performance is good is extremely urgent.
Summary of the invention
It is an object of the invention to provide the synthetic method of a kind of nanometer of three-way catalyst powder body, making it have technology difficulty low, it is easy to amplify, regulation and control are convenient, and the feature that precious metal atom utilization rate is high and catalytic performance is good, thus being easily achieved large-scale industrial production.
Technical scheme is as follows:
A kind of method of synthesis nanometer three-way catalyst powder body, it is characterised in that the method carries out as follows:
1) adding catalyst precursors in alcoholic solvent, i.e. Pd, the compound of one or more noble metals in Pt, Rh and Ir, surfactant and carrier, the total mol concentration of precious metal chemical complex is 0.0001～1mol/L；The total mass concentration of surfactant is 0-5 gram/ml solvent；The ratio of the gross mass of carrier and the gross mass of the noble metal in added precious metal chemical complex is 5:1～10000:1；
2) add the alcoholic solution of reducing agent when temperature is 60～300 DEG C, the response time is 1～720 minute, obtains the turbid solution of grey black, removes solvent；The total mol concentration of added reducing agent is 0.0001-10mol/L, and reducing agent and precious metal chemical complex mol ratio are 0:1-100:1；
3) by products therefrom ethanol or water washing, a nanometer three-way catalyst powder body can after drying, be obtained.
The method of another kind of synthesis nanometer three-way catalyst powder body provided by the invention, it is characterised in that the method carries out as follows:
1) in alcoholic solvent, carrier is added；
2) 60～300 DEG C it are warming up to, add the alcoholic solution of one or more precious metal chemical complexs in Pd, Pt, Rh, Ir, in the solution that gained contains carrier and precious metal chemical complex, the total mol concentration of precious metal chemical complex is 0.0001～1mol/L solvent, reaction time range is 1～720 minute, obtain the turbid solution of grey black, remove solvent；
3) by products therefrom ethanol or water washing, a nanometer three-way catalyst powder body can after drying, be obtained.
Solvent adopt methanol, ethanol, ethylene glycol, 1-propanol, 2-propanol, glycerol, 1, ammediol, 1,2-propylene glycol, n-butyl alcohol, the tert-butyl alcohol, 2-butanol, 1,2-butanediol, 1,3 butylene glycol, 1,4-butanediol, 1,2,3-butantriols, 1, one or more alcoholic solvents formed in 2,4-butantriols, erythrol.
Precious metal chemical complex adopts the nitrate of palladium, platinum, rhodium, iridium noble metal metal, the acetylacetonate of acetate or described metal or chloride, and the coordination compound containing corresponding precious metal element or the acid containing its complex ion, alkali or salt.
Reducing agent adopts one or more in sodium borohydride, monoborane-tert-butylamine complex, ammonia borine, three tertiary butyoxy aluminum lithiums and tri octyl phosphine.
Surfactant uses one or more in polyvinyl alcohol, Polyethylene Glycol, polyvinylpyrrolidone, cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, tetrabutyl ammonium bromide.
Described carrier adopts aluminium oxide, cerium oxide, zirconium oxide, cerium zirconium sosoloid, lanthana, yittrium oxide, titanium oxide, niobium oxide, hafnium oxide, nickel oxide, ferrum oxide, cesium fluoride, strontium fluoride, cesium carbonate, strontium carbonate, magnesium oxide, Afluon (Asta), magnesium carbonate, silicon oxide, calcium fluoride, potassium fluoride, calcium carbonate, calcium oxide, calcium hydroxide, Barium monoxide, barium fluoride, brium carbonate, potassium carbonate, sulphuric acid oxygen lanthanum, Cs2O, strontium oxide, potassium oxide, Cesium hydrate., Strontium hydrate., potassium hydroxide, barium hydroxide, hydrated ferric oxide., the mixed carrier that one or more in nickel hydroxide form.
The present invention is compared with prior art, have the following advantages and salience effect: the present invention adopts precious metal chemical complex such as nitrate, acetate, chloride, acetylacetonate and other common compounds to be raw material, and alcoholic solvent such as methanol, ethanol, ethylene glycol, 1-propanol, 2-propanol, glycerol, 1, ammediol, 1,2-propylene glycol, n-butyl alcohol, the tert-butyl alcohol, 2-butanol, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 1,2,3-butantriol, 1,2,4-butantriols, erythrol are solvent, adopt simple approach to prepare a nanometer three-way catalyst.Noble metal granule pattern in product is homogeneous, good dispersion, narrow diameter distribution, and composition, size adjustable controlled.The method adopts " one kettle way " synthetic catalyst powder body, and technique is simple, it is easy to amplifies and produces, and raw material is cheap and easy to get；Products obtained therefrom also has relatively larger performance regulation and control space, as passed through to regulate the composition of noble metal, namely in synthesis, the ratio of different noble metals makes its catalytic performance adjusted, it is also possible to regulate activity and the stability of nanometer three-way catalyst by regulating and controlling the composition of carrier.In a word, the invention provides a kind of simple method of synthesis nanometer three-way catalyst powder body, be very suitable for industrial amplification production, there is extremely wide application prospect.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope figure of palladium three-way catalyst powder body.
Fig. 2 is the transmission electron microscope figure of Rh catalyst powder.
Fig. 3 is the projection electron microscope figure of Pd-Rh three-way catalyst powder body.
Fig. 4 is Pd/Al2O3Conversion ratio-the temperature curve of three-way catalyst performance test.
Detailed description of the invention
The method of a kind of synthesis nanometer three-way catalyst powder body provided by the invention, it specifically includes as follows:
1) catalyst precursor solution is prepared: the compound of one or more noble metals in addition surfactant, carrier and Pd, Pt, Rh and Ir in alcoholic solvent, the total mol concentration of the compound of noble metal is 0.0001～1mol/L；The total mass concentration of surfactant is 0-5 gram/ml solvent；The ratio of the gross mass of carrier and the gross mass of the noble metal in added precious metal chemical complex is 5:1～10000:1；
2) add the alcoholic solution of reducing agent when temperature is 60～300 DEG C, the response time is 1～720 minute, obtains the turbid solution of grey black, removes solvent；The total mol concentration of added reducing agent is 0.0001-10mol/L, and reducing agent and precious metal chemical complex mol ratio are 0:1-100:1；
3) by products therefrom ethanol or water washing, a nanometer three-way catalyst powder body after drying, is obtained.
The method that present invention also offers another kind of synthesis nanometer three-way catalyst powder body, it is characterised in that the method carries out as follows:
1) in alcoholic solvent, carrier is first added, then heat to 60～300 DEG C, add the alcoholic solution of the compound of one or more noble metals in Pd, Pt, Rh and Ir, in the solution that gained contains carrier and precious metal chemical complex, the total mol concentration of precious metal chemical complex is 0.0001～1mol/L, response time is 1～720 minute, obtain the turbid solution of grey black, remove solvent；
3) by products therefrom ethanol or water washing, a nanometer three-way catalyst powder body can after drying, be obtained.
3. the method for the synthesis nanometer three-way catalyst described in claim 1 or 2, it is characterized in that: alcoholic solvent adopt methanol, ethanol, ethylene glycol, 1-propanol, 2-propanol, glycerol, 1,3-PD, 1,2-PD, n-butyl alcohol, the tert-butyl alcohol, 2-butanol, 1,2-butanediol, 1,3-butanediol, BDO, 1,2,3-butantriol, the mixing of one or more in BT and erythrol.
In said method, described precious metal chemical complex adopts palladium, platinum, rhodium, the nitrate of iridium noble metal, acetate or the acetylacetonate of described metal or chloride, and the coordination compound containing corresponding precious metal element or the acid containing its complex ion, alkali or salt.Described reducing agent adopts one or more in sodium borohydride, monoborane-tert-butylamine complex, ammonia borine, three tertiary butyoxy aluminum lithiums and tri octyl phosphine.Surfactant uses one or more in polyvinyl alcohol, Polyethylene Glycol, polyvinylpyrrolidone, cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, tetrabutyl ammonium bromide.Described carrier adopts aluminium oxide, cerium oxide, zirconium oxide, cerium zirconium sosoloid, lanthana, yittrium oxide, titanium oxide, niobium oxide, hafnium oxide, nickel oxide, ferrum oxide, cesium fluoride, strontium fluoride, cesium carbonate, strontium carbonate, magnesium oxide, Afluon (Asta), magnesium carbonate, silicon oxide, calcium fluoride, potassium fluoride, calcium carbonate, calcium oxide, calcium hydroxide, Barium monoxide, barium fluoride, brium carbonate, potassium carbonate, sulphuric acid oxygen lanthanum, Cs2O, strontium oxide, potassium oxide, Cesium hydrate., Strontium hydrate., potassium hydroxide, barium hydroxide, one or more mixed carriers formed in hydrated ferric oxide. and nickel hydroxide.
Enumerate several specific embodiment below, to further appreciate that specific embodiment of the invention.
Embodiment 1:
Take 10ml ethylene glycol and add 5g aluminium oxide, the chlorine palladium acid sodium of 3g, be heated to 160 DEG C, keep temperature 6h, precipitate with washing with alcohol gained after pouring out ethylene glycol solvent, dry at 40 DEG C, it is possible to obtain full Pd nanometer of three-way catalyst powder body.
Embodiment 2:
Take the 10ml tert-butyl alcohol and add 0.1g cobalt oxide, 0.3mg chlorine palladium acid sodium, be heated to 300 DEG C, keep temperature 12h, be cooled to room temperature, after centrifugal, by gained precipitation washing with alcohol, dry, full Pd nanometer of three-way catalyst powder body can be obtained.
Embodiment 3:
Take 10ml glycerol and add 0.1g cerium zirconium sosoloid, the palladium acetylacetonate of 0.3g and 50g polyvinylpyrrolidone, it is heated to 60 DEG C, add the ethylene glycol solution of the borine tert-butylamine of 100ml0.0001mol/L, keep temperature 1min, gained precipitation is washed with water after pouring out alcoholic solvent, dry at 80 DEG C, it is possible to obtain full Pd nanometer of three-way catalyst powder body.
Embodiment 4:
Take 10ml n-butyl alcohol and add 2.5g cerium oxide and 2.5g lanthana, the radium chloride of 1.3g and 1.5g palladium acetylacetonate, it is heated to 300 DEG C, add the 1,3 butylene glycol solution of the sodium borohydride of 10ml10mol/L, keep temperature 12h, filter, precipitate with water and washing with alcohol gained, dry at 80 DEG C, it is possible to obtain PdRh nanometer of three-way catalyst powder body.
Embodiment 5:
Taking 10ml1, ammediol adds 4g ferrum oxide and 3.5g magnesium oxide, 1.5g chlorine palladium acid sodium and 2g acetylacetone,2,4-pentanedione platinum, and 50g cetyl trimethylammonium bromide, it is heated to 300 DEG C, adds the 1,2-PD solution of 10L0.0001mol/L monoborane-tert-butylamine complex, keep temperature 1min, after being cooled to room temperature, pour out alcoholic solvent, precipitate with washing with alcohol gained, dry, a nanometer three-way catalyst powder body can be obtained.
Embodiment 6:
Take 5ml1,3-butanediol and add 5g aluminium oxide, be heated to 60 DEG C, add 5ml containing the 1 of 2.2g palladium, 3-butanediol solution, keeps temperature 12h, pours out 1, by washing with alcohol gained precipitation after 3-butanediol solvent, dry at 80 DEG C, it is possible to obtain full Pd nanometer of three-way catalyst powder body.
Embodiment 7:
Take 1ml ethylene glycol and add 2.5g calcium hydroxide, 5g hafnium oxide, be heated to 240 DEG C, add the 9ml ethylene glycol solution containing 1.5g palladium acetylacetonate and 1.5g iridium chloride, keep temperature 12h, wash gained precipitation after pouring out ethylene glycol solvent with water, dry, it is possible to obtain a nanometer three-way catalyst powder body.
Embodiment 8:
Taking 9ml1,2,3-butantriols add 0.1g niobium oxide, are heated to 300 DEG C, add the 1ml ethylene glycol solution containing 0.3mg palladium acetylacetonate, keep temperature 1min, by washing with alcohol gained precipitation after centrifugal, dry at 80 DEG C, it is possible to obtain catalyst powder.
Embodiment 9:
Measure 3ml n-butyl alcohol and add 0.1g nickel oxide, be heated to 60 DEG C, add the 7ml glycerin solution containing 0.4mg acetylacetone,2,4-pentanedione rhodium, keep temperature 12h, filter, precipitate with water and washing with alcohol gained, dry, it is possible to obtain catalyst powder.
Embodiment 10:
Measuring 5ml1, ammediol adds 3g cerium zirconium sosoloid and 4.5g cobalt oxide, is heated to 300 DEG C, add the 5ml normal propyl alcohol solution containing 1.5g chlorine palladium acid sodium and 2g acetylacetone,2,4-pentanedione rhodium, keep temperature 1min, centrifugation, precipitate with washing with alcohol gained, dry at 80 DEG C, it is possible to obtain catalyst powder.
Claims (7)
1. the method for a synthesis nanometer three-way catalyst powder body, it is characterised in that the method carries out as follows:
1) catalyst precursor solution is prepared: the compound of one or more noble metals in addition surfactant, carrier and Pd, Pt, Rh and Ir in alcoholic solvent, the total mol concentration of precious metal chemical complex is 0.0001～1mol/L；The total mass concentration of surfactant is 0-5 gram/ml solvent；The ratio of the gross mass of carrier and the gross mass of the noble metal in added precious metal chemical complex is 5:1～10000:1；
2) add the alcoholic solution of reducing agent when temperature is 60～300 DEG C, the response time is 1～720 minute, obtains the turbid solution of grey black, removes solvent；The total mol concentration of added reducing agent is 0.0001-10mol/L, and reducing agent and precious metal chemical complex mol ratio are 0:1-100:1；
3) by products therefrom ethanol or water washing, a nanometer three-way catalyst powder body after drying, is obtained.
2. the method for a synthesis nanometer three-way catalyst powder body, it is characterised in that the method carries out as follows:
1) in alcoholic solvent, carrier is first added, then heat to 60～300 DEG C, add the alcoholic solution of one or more precious metal chemical complexs in Pd, Pt, Rh and Ir, in the solution that gained contains carrier and precious metal chemical complex, the total mol concentration of precious metal chemical complex is 0.0001～1mol/L solvent, response time is 1～720 minute, obtain the turbid solution of grey black, remove solvent；
3) by products therefrom ethanol or water washing, a nanometer three-way catalyst powder body can after drying, be obtained.
3. the method for the synthesis nanometer three-way catalyst described in claim 1 or 2, it is characterized in that: alcoholic solvent adopt methanol, ethanol, ethylene glycol, 1-propanol, 2-propanol, glycerol, 1,3-PD, 1,2-PD, n-butyl alcohol, the tert-butyl alcohol, 2-butanol, 1,2-butanediol, 1,3-butanediol, BDO, 1,2,3-butantriol, one or more mixed solutions formed in BT and erythrol.
4. the method for the synthesis nanometer three-way catalyst described in claim 1 or 2, it is characterized in that: described precious metal chemical complex adopts palladium, platinum, rhodium, the nitrate of iridium noble metal metal, acetate, or the acetylacetonate of described metal or chloride, and the coordination compound containing corresponding precious metal element or the acid containing its complex ion, alkali or salt.
5. the method for the synthesis nanometer three-way catalyst described in claim 1 or 2, it is characterised in that: described reducing agent adopts one or more in sodium borohydride, monoborane-tert-butylamine complex, ammonia borine, three tertiary butyoxy aluminum lithiums and tri octyl phosphine.
6. the method for the synthesis nanometer three-way catalyst described in claim 1 or 2, it is characterised in that: surfactant uses one or more in polyvinyl alcohol, Polyethylene Glycol, polyvinylpyrrolidone, cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, tetrabutyl ammonium bromide.
7. the method for the synthesis nanometer three-way catalyst described in claim 1 or 2, it is characterized in that: described carrier adopts aluminium oxide, cerium oxide, zirconium oxide, cerium zirconium sosoloid, lanthana, yittrium oxide, titanium oxide, niobium oxide, hafnium oxide, nickel oxide, ferrum oxide, cesium fluoride, strontium fluoride, cesium carbonate, strontium carbonate, magnesium oxide, Afluon (Asta), magnesium carbonate, silicon oxide, calcium fluoride, potassium fluoride, calcium carbonate, calcium oxide, calcium hydroxide, Barium monoxide, barium fluoride, brium carbonate, potassium carbonate, sulphuric acid oxygen lanthanum, Cs2O, strontium oxide, potassium oxide, Cesium hydrate., Strontium hydrate., potassium hydroxide, barium hydroxide, one or more mixed carriers formed in hydrated ferric oxide. and nickel hydroxide.
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