CN105289461A - Formula and preparing method of automobile three-way catalyst - Google Patents
Formula and preparing method of automobile three-way catalyst Download PDFInfo
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- CN105289461A CN105289461A CN201510686642.6A CN201510686642A CN105289461A CN 105289461 A CN105289461 A CN 105289461A CN 201510686642 A CN201510686642 A CN 201510686642A CN 105289461 A CN105289461 A CN 105289461A
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- 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
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- 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
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/10—Internal combustion engine [ICE] based vehicles
- Y02T10/12—Improving ICE efficiencies
Abstract
The invention discloses a formula and preparing method of an automobile three-way catalyst. The automobile three-way catalyst is characterized by being prepared from, by weight, 80% to 90% of porous ceramic, 5% to 10% of adsorbing agents and 5% to 10% of catalysts; the porous ceramic is prepared from, by weight, 90 parts to 100 parts of alumina sol, 40 parts to 60 parts of micro-nano-grade alpha-Al2O3, 20 parts to 30 parts of pore-forming agents, 0 part to 5 parts of binding agents, 2 parts to 5 parts of adhesion agents and 250 parts to 350 parts of an acid solution with the pH of 3-4; the adsorbing agents comprise single-crystal magnesium oxide. According to the formula and preparing method of the automobile three-way catalyst, the single-crystal magnesium oxide replaces traditional aluminum oxide to serve as the adsorbing agents, and the purifying capacity is 2-3 times that of the aluminum oxide; the porous ceramic with even pores and the high pore forming rate is prepared with an alumina sol/gel method in cooperation with the inorganic salt hole forming agents, the specific surface area of the porous ceramic is large accordingly, the number of catalytic activation loci is large, and purifying capacity is high.
Description
Technical field
The present invention relates to a kind of automobile three-way catalysts formula and preparation method thereof, belong to environment protection catalytic technical field.
Background technology
Ternary catalyzing unit, is mounted in most important outer purifier in automobile exhaust system, and the pernicious gases such as CO, HC and NOx that vehicle exhaust can be discharged by it change harmless carbon dioxide, water and nitrogen into by oxidation and reduction.When the vehicle exhaust of high temperature is by purifier, cleanser in ternary catalyzing unit will strengthen the activity of CO, HC and NOx tri-kinds of gases, impel it to carry out certain oxidationreduction chemical reaction, wherein CO is at high temperature oxidized into colourless, nontoxic carbon dioxide; HC compound is at high temperature oxidized to water and carbon dioxide; NOx is reduced into nitrogen and oxygen.Three kinds of pernicious gases become innocuous gas, and vehicle exhaust is purified.
The structure of purifier comprises carrier (i.e. porous ceramics) and load at supported catalyst, and the hole of carrier is more much more even, then effective adsorption surface area of carrier is larger, and detergent power is stronger.The pore former of current carrier is generally organic pore former, as natural fiber, high molecular polymer and organic acid etc., organic pore former is decomposed under far below carrier sintering temperature, hole is left after decomposition, these holes, especially some apertures, easily close when high temperature sintering is below shaping, cause the porosity of carrier low, catalytic capability is poor.
In addition, the adsorbent in present catalyst generally selects aluminium oxide, and the adsorbable Small molecular polar compound of aluminium oxide, as CO, HC and NOx, changes CO, HC and NOx into harmless carbon dioxide, water and nitrogen by catalyst after absorption again; But aluminium oxide exists adsorption capacity, and comparatively magnesia is poor, therefore the invention provides a kind of automobile three-way catalysts stronger to vehicle exhaust Molecular Adsorption ability formula and preparation method thereof.
Summary of the invention
The technical problem that the present invention solves is, provide a kind of become strong, stronger to the vehicle exhaust Molecular Adsorption ability automobile three-way catalysts formula of large, the detergent power of high, the effective adsorption surface area of porosity; Further, the invention provides and a kind of adopt sol-gel process preparation, adopt Small molecular inorganic salts pore-forming, become porosity high, pore-forming is even simultaneously, and Alumina gel solid content is high, preparation method to the stronger automobile three-way catalysts of vehicle exhaust Molecular Adsorption ability.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of automobile three-way catalysts formula, is characterized in that: comprising: the catalyst of the porous ceramics of 80 ~ 90wt%, the adsorbent of 5 ~ 10wt% and 5 ~ 10wt%; Described porous ceramics comprises the raw material of following weight portion: Alumina gel 90 ~ 100 parts, micro/nano level α-Al
2o
340 ~ 60 parts, pore former 20 ~ 30 parts, binding agent 0 ~ 5 part, 2 ~ 5 parts, adhesive and pH be 3 ~ 4 acid solution 250 ~ 350 parts; Described pore former is inorganic salts; Described adhesive comprises calcium sulfate; Described adsorbent comprises magnesium oxide single crystal; Described catalyst comprises metal oxide containing precious metals and rare earth oxide.
Described binding agent comprises polyvinyl alcohol.
Described pore former comprises one or more in sodium sulphate, calcium sulfate, sodium chloride, calcium chloride.
Described metal oxide containing precious metals comprises Pt oxide, Pd oxide and Rh oxide.
Described rare earth oxide comprises one or more in the oxide of lanthanum La, cerium Ce, praseodymium Pr, neodymium Nd, promethium Pm, samarium Sm, europium Eu, gadolinium Gd, terbium Tb, dysprosium Dy, holmium Ho, erbium Er, thulium Tm, ytterbium Yb, lutetium Lu, scandium Sc and yttrium Y.
A preparation method for automobile three-way catalysts, is characterized in that: comprise the following steps:
S01, the preparation of Alumina gel:
S01-1, the preparation of sodium aluminate solution: be dissolved in ultra-pure water by NaOH solid and be mixed with 5%NaOH solution, then be added in 5%NaOH solution by aluminium powder, aluminium powder adds weight: 5%NaOH liquor capacity is 4 ~ 5:100; Filter after stirring and dissolving, obtain sodium aluminate solution;
S01-2, the preparation of boehmite precipitation: by NaHCO
3solid is dissolved in ultra-pure water and gathers the NaHCO being mixed with 4 ~ 4.5%
3solution, described NaHCO
3the volume of solution is at least 3 times amount of sodium aluminate solution volume, by described NaHCO
3solution is added in described sodium aluminate solution while stirring, and after having added, heating is also stirred at least after 30min simultaneously, filters, obtains boehmite precipitation;
S01-3, cleaning boehmite precipitation: after ultra-pure water cleaning, boehmite precipitation is put into ultra-pure water, add Cation adsorption resin adsorption at least after 10min, ultra-pure water cleans, then boehmite precipitation is put into ultra-pure water, add Anion-adsorption resin adsorption at least after 10min, ultra-pure water cleaning is neutral to cleaning fluid, dry;
S01-4, acid adding prepares Alumina gel: join in the salpeter solution of 1mol/L by dried boehmite precipitation, and heating stirring and dissolving obtains Alumina gel, and sour aluminum ratio is 0.08 ~ 0.20;
S02, the preparation of high solids content Alumina gel: add micro/nano level α-Al in the Alumina gel of S01-4
2o
3, after heating for dissolving, obtain the Alumina gel that solid content reaches 60 ~ 65%;
S03, in the high solids content Alumina gel of S02, add pore former, binding agent and adhesive, after heating stirs, inject mould cast molding, then put into vacuum drying chamber vacuum outgas and drying, obtain preliminary forming ceramic, vacuum drying temperature is 50 ~ 70 DEG C;
S04, unsticking and sintering: by described just one-step forming ternary catalyzing unit in atmosphere through 500 ~ 600 DEG C of unstickings at least 1 hour, then put into high temperature furnace through 1000 ~ 1100 DEG C of sintering at least 1 hour, then cool, obtain post forming pottery;
S05, it is in the acid solution of 3 ~ 4 that described post forming pottery is put into pH, adds thermal response at least 3 hours, then takes out, and ultra-pure water cleaning, to neutral, dried, obtained porous ceramics.
S06, magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide are made coating slurry, again described porous ceramics is flooded 3 ~ 10 minutes in described coating slurry, roasting 3 ~ 5 hours at 700 ~ 800 DEG C after drying, again under 450 ~ 500 DEG C of conditions, with hydrogen reducing at least 4 hours, obtain ternary catalyzing unit.
In S01-2, heating-up temperature is 80 ~ 85 DEG C.
The addition of described Cation adsorption resin and Anion-adsorption resin is 1/10 of at least boehmite precipitation weight.
Described sour aluminum ratio is 0.10 ~ 0.12.
Heating-up temperature in S02 is 50 ~ 70 DEG C.
Described acid solution is salpeter solution.
Acid aluminum ratio refers to the ratio of the amount of substance of acid solution and the amount of substance of boehmite precipitation.
The preparation method of described coating slurry is, get magnesium oxide single crystal, metal oxide containing precious metals, rare earth oxide and water, grinding in ball grinder at least 6 hours, the addition of water was 300 ~ 500 times of the total amount of described magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide.
A kind of automobile three-way catalysts formula provided by the invention and preparation method thereof, replaces traditional aluminium oxide as adsorbent with magnesium oxide single crystal, and the ability of magnesium oxide single crystal adsorption vehicle tail gas molecule is stronger, and detergent power is 2 ~ 3 times of aluminium oxide; Pore former is the setting of inorganic salts, and inorganic salts fusing point is high, also can not melt when high temperature sintering, rear acid dissolve inorganic salts are sintered, obtain porous ceramics, the porous ceramics prepared with inorganic salts, even pore distribution, specific area are large, catalytic activation site is many, detergent power is strong; Alumina gel-gel method is in conjunction with the setting of inorganic salts pore former, and the specific area further increasing porous ceramics is large, and pore former is uniformly dispersed in high solids content Alumina gel, even pore distribution during pore-forming, becomes porosity up to 60%; Micro/nano level α-Al
2o
3interpolation, make Alumina gel solid content high and easily flow; Adhesive is the setting of calcium sulfate, makes porous ceramics form acidic alumina in the process of preparation, is applicable to decomposing pore former in acid condition, thus forms porous ceramics; The setting of Cation adsorption resin and Anion-adsorption resin, the cation in adsorbable cleaning boehmite precipitation and anion, be convenient to fast that boehmite precipitation cleaning is extremely neutral; In addition, the setting of magnesium oxide single crystal, also has guard catalyst not by the effect of sulfur poisoning, further enhancing detergent power and the service life of ternary catalyzing unit.A kind of automobile three-way catalysts formula provided by the invention and preparation method thereof, adopt magnesium oxide single crystal to replace traditional aluminium oxide as adsorbent, detergent power is 2 ~ 3 times of aluminium oxide; Adopt Alumina gel-gel method to prepare porous nickel in conjunction with inorganic salts pore former, become porosity much higher hole pottery, make porous ceramics specific area large, catalytic activation site is many, and detergent power is strong.
Detailed description of the invention
Below the present invention is further described.
embodiment 1:
A kind of automobile three-way catalysts formula, is characterized in that: comprising: the catalyst of the porous ceramics of 80wt%, the adsorbent of 10wt% and 10wt%; Described porous ceramics comprises the raw material of following weight portion: Alumina gel 90 parts, micro/nano level α-Al
2o
340 parts, pore former 20 parts, binding agent 0 part, 2 parts, adhesive and pH be 3 acid solution 250 parts; Described pore former is inorganic salts; Described adhesive comprises calcium sulfate; Described adsorbent comprises magnesium oxide single crystal; Described catalyst comprises metal oxide containing precious metals and rare earth oxide.
Described binding agent comprises polyvinyl alcohol.
Described pore former comprises one or more in sodium sulphate, calcium sulfate, sodium chloride, calcium chloride.
Described metal oxide containing precious metals comprises Pt oxide, Pd oxide and Rh oxide.
Described rare earth oxide comprises one or more in the oxide of lanthanum La, cerium Ce, praseodymium Pr, neodymium Nd, promethium Pm, samarium Sm, europium Eu, gadolinium Gd, terbium Tb, dysprosium Dy, holmium Ho, erbium Er, thulium Tm, ytterbium Yb, lutetium Lu, scandium Sc and yttrium Y.
A preparation method for automobile three-way catalysts, is characterized in that: comprise the following steps:
S01, the preparation of Alumina gel:
S01-1, the preparation of sodium aluminate solution: be dissolved in ultra-pure water by NaOH solid and be mixed with 5%NaOH solution, then be added in 5%NaOH solution by aluminium powder, aluminium powder adds weight: 5%NaOH liquor capacity is 4:100; Filter after stirring and dissolving, obtain sodium aluminate solution;
S01-2, the preparation of boehmite precipitation: by NaHCO
3solid is dissolved in ultra-pure water and gathers the NaHCO being mixed with 4%
3solution, described NaHCO
3the volume of solution is 3 times amount of sodium aluminate solution volume, by described NaHCO
3solution is added in described sodium aluminate solution while stirring, and after having added, heating also, after stirring 30min simultaneously, is filtered, obtained boehmite precipitation;
S01-3, cleaning boehmite precipitation: after ultra-pure water cleaning, boehmite precipitation is put into ultra-pure water, after adding Cation adsorption resin adsorption 10min, ultra-pure water cleans, then boehmite precipitation is put into ultra-pure water, after adding Anion-adsorption resin adsorption 10min, ultra-pure water cleaning is neutral to cleaning fluid, dry;
S01-4, acid adding prepares Alumina gel: join in the salpeter solution of 1mol/L by dried boehmite precipitation, and heating stirring and dissolving obtains Alumina gel, and sour aluminum ratio is 0.08;
S02, the preparation of high solids content Alumina gel: add micro/nano level α-Al in the Alumina gel of S01-4
2o
3, after heating for dissolving, obtain the Alumina gel that solid content reaches 60%;
S03, adds pore former, binding agent and adhesive in the high solids content Alumina gel of S02, injects mould cast molding after heating stirs, and then put into vacuum drying chamber vacuum outgas and drying, obtain preliminary forming ceramic, vacuum drying temperature is 50 DEG C;
S04, unsticking and sintering: by described just one-step forming ternary catalyzing unit in atmosphere through 500 DEG C of unstickings 1 hour, then put into high temperature furnace through 1000 DEG C of sintering 1 hour, then cool, obtain post forming pottery;
S05, it is in the acid solution of 3 that described post forming pottery is put into pH, adds thermal response at least 3 hours, then takes out, and ultra-pure water cleaning, to neutral, dried, obtained porous ceramics;
S06, makes coating slurry by magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide, then is flooded 3 minutes in described coating slurry by described porous ceramics, roasting 3 hours at 700 DEG C after drying, again under 450 DEG C of conditions, with hydrogen reducing 4 hours, obtain ternary catalyzing unit.
In S01-2, heating-up temperature is 80 DEG C.
The addition of described Cation adsorption resin and Anion-adsorption resin is 1/10 of boehmite precipitation weight.
Heating-up temperature in S02 is 50 DEG C.
Described acid solution is salpeter solution.
The preparation method of described coating slurry is get magnesium oxide single crystal, metal oxide containing precious metals, rare earth oxide and water, and grinding in ball grinder 6 hours, the addition of water was 300 times of the total amount of described magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide.
embodiment 2:
A kind of automobile three-way catalysts formula, is characterized in that: comprising: the catalyst of the porous ceramics of 90wt%, the adsorbent of 5wt% and 5wt%; Described porous ceramics comprises the raw material of following weight portion: Alumina gel 100 parts, micro/nano level α-Al
2o
360 parts, pore former 30 parts, binding agent 5 parts, 5 parts, adhesive and pH be 4 acid solution 350 parts; Described pore former is inorganic salts; Described adhesive comprises calcium sulfate; Described adsorbent comprises magnesium oxide single crystal; Described catalyst comprises metal oxide containing precious metals and rare earth oxide.
Described binding agent comprises polyvinyl alcohol.
Described pore former comprises one or more in sodium sulphate, calcium sulfate, sodium chloride, calcium chloride.
Described metal oxide containing precious metals comprises Pt oxide, Pd oxide and Rh oxide.
Described rare earth oxide comprises one or more in the oxide of lanthanum La, cerium Ce, praseodymium Pr, neodymium Nd, promethium Pm, samarium Sm, europium Eu, gadolinium Gd, terbium Tb, dysprosium Dy, holmium Ho, erbium Er, thulium Tm, ytterbium Yb, lutetium Lu, scandium Sc and yttrium Y.
A preparation method for automobile three-way catalysts, is characterized in that: comprise the following steps:
S01, the preparation of Alumina gel:
S01-1, the preparation of sodium aluminate solution: be dissolved in ultra-pure water by NaOH solid and be mixed with 5%NaOH solution, then be added in 5%NaOH solution by aluminium powder, aluminium powder adds weight: 5%NaOH liquor capacity is 5:100; Filter after stirring and dissolving, obtain sodium aluminate solution;
S01-2, the preparation of boehmite precipitation: by NaHCO
3solid is dissolved in ultra-pure water and gathers the NaHCO being mixed with 4.5%
3solution, described NaHCO
3the volume of solution is 3.5 times amount of sodium aluminate solution volume, by described NaHCO
3solution is added in described sodium aluminate solution while stirring, and after having added, heating also, after stirring 40min simultaneously, is filtered, obtained boehmite precipitation;
S01-3, cleaning boehmite precipitation: after ultra-pure water cleaning, boehmite precipitation is put into ultra-pure water, after adding Cation adsorption resin adsorption 15min, ultra-pure water cleans, then boehmite precipitation is put into ultra-pure water, after adding Anion-adsorption resin adsorption 15min, ultra-pure water cleaning is neutral to cleaning fluid, dry;
S01-4, acid adding prepares Alumina gel: join in the salpeter solution of 1mol/L by dried boehmite precipitation, and heating stirring and dissolving obtains Alumina gel, and sour aluminum ratio is 0.20;
S02, the preparation of high solids content Alumina gel: add micro/nano level α-Al in the Alumina gel of S01-4
2o
3, after heating for dissolving, obtain the Alumina gel that solid content reaches 65%;
S03, adds pore former, binding agent and adhesive in the high solids content Alumina gel of S02, injects mould cast molding after heating stirs, and then put into vacuum drying chamber vacuum outgas and drying, obtain preliminary forming ceramic, vacuum drying temperature is 0 DEG C;
S04, unsticking and sintering: by described just one-step forming ternary catalyzing unit in atmosphere through 600 DEG C of unstickings 1.5 hours, then put into high temperature furnace through 100 DEG C of sintering 1.5 hours, then cool, obtain post forming pottery;
S05, it is in the acid solution of 4 that described post forming pottery is put into pH, adds thermal response 4 hours, then takes out, and ultra-pure water cleaning, to neutral, dried, obtained porous ceramics;
S06, makes coating slurry by magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide, then is flooded 10 minutes in described coating slurry by described porous ceramics, roasting 5 hours at 800 DEG C after drying, again under 500 DEG C of conditions, with hydrogen reducing 4.5, obtain ternary catalyzing unit.
In S01-2, heating-up temperature is 85 DEG C.
The addition of described Cation adsorption resin and Anion-adsorption resin is 1/8 of boehmite precipitation weight.
Heating-up temperature in S02 is 70 DEG C.
Described acid solution is salpeter solution.
The preparation method of described coating slurry is get magnesium oxide single crystal, metal oxide containing precious metals, rare earth oxide and water, and grinding in ball grinder 6.5 hours, the addition of water was 500 times of the total amount of described magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide.
embodiment 3:
A kind of automobile three-way catalysts formula, is characterized in that: comprising: the catalyst of the porous ceramics of 85wt%, the adsorbent of 5wt% and 10wt%; Described porous ceramics comprises the raw material of following weight portion: Alumina gel 95 parts, micro/nano level α-Al
2o
350 parts, pore former 25 parts, binding agent 2 parts, 3 parts, adhesive and pH be 3 acid solution 300 parts; Described pore former is inorganic salts; Described adhesive comprises calcium sulfate; Described adsorbent comprises magnesium oxide single crystal; Described catalyst comprises metal oxide containing precious metals and rare earth oxide.
Described binding agent comprises polyvinyl alcohol.
Described pore former comprises one or more in sodium sulphate, calcium sulfate, sodium chloride, calcium chloride.
Described metal oxide containing precious metals comprises Pt oxide, Pd oxide and Rh oxide.
Described rare earth oxide comprises one or more in the oxide of lanthanum La, cerium Ce, praseodymium Pr, neodymium Nd, promethium Pm, samarium Sm, europium Eu, gadolinium Gd, terbium Tb, dysprosium Dy, holmium Ho, erbium Er, thulium Tm, ytterbium Yb, lutetium Lu, scandium Sc and yttrium Y.
A preparation method for automobile three-way catalysts, is characterized in that: comprise the following steps:
S01, the preparation of Alumina gel:
S01-1, the preparation of sodium aluminate solution: be dissolved in ultra-pure water by NaOH solid and be mixed with 5%NaOH solution, then be added in 5%NaOH solution by aluminium powder, aluminium powder adds weight: 5%NaOH liquor capacity is 4.5:100; Filter after stirring and dissolving, obtain sodium aluminate solution;
S01-2, the preparation of boehmite precipitation: by NaHCO
3solid is dissolved in ultra-pure water and gathers the NaHCO being mixed with 4.2%
3solution, described NaHCO
3the volume of solution is 4 times amount of sodium aluminate solution volume, by described NaHCO
3solution is added in described sodium aluminate solution while stirring, and after having added, heating also, after stirring 50min simultaneously, is filtered, obtained boehmite precipitation;
S01-3, cleaning boehmite precipitation: after ultra-pure water cleaning, boehmite precipitation is put into ultra-pure water, after adding Cation adsorption resin adsorption 20min, ultra-pure water cleans, then boehmite precipitation is put into ultra-pure water, after adding Anion-adsorption resin adsorption 20min, ultra-pure water cleaning is neutral to cleaning fluid, dry;
S01-4, acid adding prepares Alumina gel: join in the salpeter solution of 1mol/L by dried boehmite precipitation, and heating stirring and dissolving obtains Alumina gel, and sour aluminum ratio is 0.10;
S02, the preparation of high solids content Alumina gel: add micro/nano level α-Al in the Alumina gel of S01-4
2o
3, after heating for dissolving, obtain the Alumina gel that solid content reaches 63%;
S03, adds pore former, binding agent and adhesive in the high solids content Alumina gel of S02, injects mould cast molding after heating stirs, and then put into vacuum drying chamber vacuum outgas and drying, obtain preliminary forming ceramic, vacuum drying temperature is 60 DEG C;
S04, unsticking and sintering: by described just one-step forming ternary catalyzing unit in atmosphere through 550 DEG C of unstickings 2 hours, then put into high temperature furnace through 1050 DEG C of sintering 2 hours, then cool, obtain post forming pottery;
S05, it is in the acid solution of 3 that described post forming pottery is put into pH, adds thermal response 5 hours, then takes out, and ultra-pure water cleaning, to neutral, dried, obtained porous ceramics;
S06, makes coating slurry by magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide, more described porous ceramics is flooded 5 clocks in described coating slurry, after drying when 750 roasting 4, again under 480 DEG C of conditions, with hydrogen reducing 5 hours, obtain ternary catalyzing unit.
In S01-2, heating-up temperature is 82 DEG C.
The addition of described Cation adsorption resin and Anion-adsorption resin is 1/10 of boehmite precipitation weight.
Heating-up temperature in S02 is 60 DEG C.
Described acid solution is salpeter solution.
The preparation method of described coating slurry is get magnesium oxide single crystal, metal oxide containing precious metals, rare earth oxide and water, and grinding in ball grinder 7 hours, the addition of water was 400 times of the total amount of described magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide.
embodiment 4:
A kind of automobile three-way catalysts formula, is characterized in that: comprising: the catalyst of the porous ceramics of 88wt%, the adsorbent of 6wt% and 6wt%; Described porous ceramics comprises the raw material of following weight portion: Alumina gel 92 parts, micro/nano level α-Al
2o
345 parts, pore former 28 parts, binding agent 4 parts, 4 parts, adhesive and pH be 4 acid solution 350 parts; Described pore former is inorganic salts; Described adhesive comprises calcium sulfate; Described adsorbent comprises magnesium oxide single crystal; Described catalyst comprises metal oxide containing precious metals and rare earth oxide.
Described binding agent comprises polyvinyl alcohol.
Described pore former comprises one or more in sodium sulphate, calcium sulfate, sodium chloride, calcium chloride.
Described metal oxide containing precious metals comprises Pt oxide, Pd oxide and Rh oxide.
Described rare earth oxide comprises one or more in the oxide of lanthanum La, cerium Ce, praseodymium Pr, neodymium Nd, promethium Pm, samarium Sm, europium Eu, gadolinium Gd, terbium Tb, dysprosium Dy, holmium Ho, erbium Er, thulium Tm, ytterbium Yb, lutetium Lu, scandium Sc and yttrium Y.
A preparation method for automobile three-way catalysts, is characterized in that: comprise the following steps:
S01, the preparation of Alumina gel:
S01-1, the preparation of sodium aluminate solution: be dissolved in ultra-pure water by NaOH solid and be mixed with 5%NaOH solution, then be added in 5%NaOH solution by aluminium powder, aluminium powder adds weight: 5%NaOH liquor capacity is 4:100; Filter after stirring and dissolving, obtain sodium aluminate solution;
S01-2, the preparation of boehmite precipitation: by NaHCO
3solid is dissolved in ultra-pure water and gathers the NaHCO being mixed with 4.3%
3solution, described NaHCO
3the volume of solution is 3.2 times amount of sodium aluminate solution volume, by described NaHCO
3solution is added in described sodium aluminate solution while stirring, and after having added, heating also, after stirring 60min simultaneously, is filtered, obtained boehmite precipitation;
S01-3, cleaning boehmite precipitation: after ultra-pure water cleaning, boehmite precipitation is put into ultra-pure water, after adding Cation adsorption resin adsorption 25min, ultra-pure water cleans, then boehmite precipitation is put into ultra-pure water, after adding Anion-adsorption resin adsorption 25min, ultra-pure water cleaning is neutral to cleaning fluid, dry;
S01-4, acid adding prepares Alumina gel: join in the salpeter solution of 1mol/L by dried boehmite precipitation, and heating stirring and dissolving obtains Alumina gel, and sour aluminum ratio is 0.12;
S02, the preparation of high solids content Alumina gel: add micro/nano level α-Al in the Alumina gel of S01-4
2o
3, after heating for dissolving, obtain the Alumina gel that solid content reaches 64%;
S03, adds pore former, binding agent and adhesive in the high solids content Alumina gel of S02, injects mould cast molding after heating stirs, and then put into vacuum drying chamber vacuum outgas and drying, obtain preliminary forming ceramic, vacuum drying temperature is 65 DEG C;
S04, unsticking and sintering: by described just one-step forming ternary catalyzing unit in atmosphere through 600 DEG C of unstickings 1 hour, then put into high temperature furnace through 1000 DEG C of sintering 1 hour, then cool, obtain post forming pottery;
S05, it is in the acid solution of 4 that described post forming pottery is put into pH, adds thermal response 6 hours, then takes out, and ultra-pure water cleaning, to neutral, dried, obtained porous ceramics;
S06, makes coating slurry by magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide, then is flooded 8 minutes in described coating slurry by described porous ceramics, roasting 3.5 hours at 780 DEG C after drying, again under 460 DEG C of conditions, with hydrogen reducing 6 hours, obtain ternary catalyzing unit.
In S01-2, heating-up temperature is 85 DEG C.
The addition of described Cation adsorption resin and Anion-adsorption resin is 1/10 of boehmite precipitation weight.
Heating-up temperature in S02 is 70 DEG C.
Described acid solution is salpeter solution.
The preparation method of described coating slurry is get magnesium oxide single crystal, metal oxide containing precious metals, rare earth oxide and water, and grinding in ball grinder 8 hours, the addition of water was 450 times of the total amount of described magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. an automobile three-way catalysts formula, is characterized in that: comprising: the catalyst of the porous ceramics of 80 ~ 90wt%, the adsorbent of 5 ~ 10wt% and 5 ~ 10wt%; Described porous ceramics comprises the raw material of following weight portion: Alumina gel 90 ~ 100 parts, micro/nano level α-Al
2o
340 ~ 60 parts, pore former 20 ~ 30 parts, binding agent 0 ~ 5 part, 2 ~ 5 parts, adhesive and pH be 3 ~ 4 acid solution 250 ~ 350 parts; Described pore former is inorganic salts; Described adhesive comprises calcium sulfate; Described adsorbent comprises magnesium oxide single crystal; Described catalyst comprises metal oxide containing precious metals and rare earth oxide.
2. a kind of automobile three-way catalysts formula according to claim 1, is characterized in that: described binding agent comprises polyvinyl alcohol.
3. a kind of automobile three-way catalysts formula according to claim 1, is characterized in that: described pore former comprises one or more in sodium sulphate, calcium sulfate, sodium chloride, calcium chloride.
4. a kind of automobile three-way catalysts formula according to claim 1, is characterized in that: described metal oxide containing precious metals comprises Pt oxide, Pd oxide and Rh oxide.
5. a kind of automobile three-way catalysts formula according to claim 1, is characterized in that: described rare earth oxide comprises one or more in the oxide of lanthanum La, cerium Ce, praseodymium Pr, neodymium Nd, promethium Pm, samarium Sm, europium Eu, gadolinium Gd, terbium Tb, dysprosium Dy, holmium Ho, erbium Er, thulium Tm, ytterbium Yb, lutetium Lu, scandium Sc and yttrium Y.
6. the preparation method of a kind of automobile three-way catalysts according to any one of claim 1 ~ 5, is characterized in that: comprise the following steps:
S01, the preparation of Alumina gel:
S01-1, the preparation of sodium aluminate solution: be dissolved in ultra-pure water by NaOH solid and be mixed with 5%NaOH solution, then be added in 5%NaOH solution by aluminium powder, aluminium powder adds weight: 5%NaOH liquor capacity is 4 ~ 5:100; Filter after stirring and dissolving, obtain sodium aluminate solution;
S01-2, the preparation of boehmite precipitation: by NaHCO
3solid is dissolved in ultra-pure water and gathers the NaHCO being mixed with 4 ~ 4.5%
3solution, described NaHCO
3the volume of solution is at least 3 times amount of sodium aluminate solution volume, by described NaHCO
3solution is added in described sodium aluminate solution while stirring, and after having added, heating is also stirred at least after 30min simultaneously, filters, obtains boehmite precipitation;
S01-3, cleaning boehmite precipitation: after ultra-pure water cleaning, boehmite precipitation is put into ultra-pure water, add Cation adsorption resin adsorption at least after 10min, ultra-pure water cleans, then boehmite precipitation is put into ultra-pure water, add Anion-adsorption resin adsorption at least after 10min, ultra-pure water cleaning is neutral to cleaning fluid, dry;
S01-4, acid adding prepares Alumina gel: join in the salpeter solution of 1mol/L by dried boehmite precipitation, and heating stirring and dissolving obtains Alumina gel, and sour aluminum ratio is 0.08 ~ 0.20;
S02, the preparation of high solids content Alumina gel: add micro/nano level α-Al in the Alumina gel of S01-4
2o
3, after heating for dissolving, obtain the Alumina gel that solid content reaches 60 ~ 65%;
S03, in the high solids content Alumina gel of S02, add pore former, binding agent and adhesive, after heating stirs, inject mould cast molding, then put into vacuum drying chamber vacuum outgas and drying, obtain preliminary forming ceramic, vacuum drying temperature is 50 ~ 70 DEG C;
S04, unsticking and sintering: by described just one-step forming ternary catalyzing unit in atmosphere through 500 ~ 600 DEG C of unstickings at least 1 hour, then put into high temperature furnace through 1000 ~ 1100 DEG C of sintering at least 1 hour, then cool, obtain post forming pottery;
S05, it is in the acid solution of 3 ~ 4 that described post forming pottery is put into pH, adds thermal response at least 3 hours, then takes out, and ultra-pure water cleaning, to neutral, dried, obtained porous ceramics;
S06, magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide are made coating slurry, again described porous ceramics is flooded 3 ~ 10 minutes in described coating slurry, roasting 3 ~ 5 hours at 700 ~ 800 DEG C after drying, again under 450 ~ 500 DEG C of conditions, with hydrogen reducing at least 4 hours, obtain ternary catalyzing unit.
7. the preparation method of a kind of automobile three-way catalysts according to claim 6, is characterized in that: in S01-2, heating-up temperature is 80 ~ 85 DEG C; Heating-up temperature in S02 is 50 ~ 70 DEG C; Described sour aluminum ratio is 0.10 ~ 0.12; .
8. the preparation method of a kind of automobile three-way catalysts according to claim 6, is characterized in that: the addition of described Cation adsorption resin and Anion-adsorption resin is 1/10 of at least boehmite precipitation weight.
9. the preparation method of a kind of automobile three-way catalysts according to claim 6, it is characterized in that: the preparation method of described coating slurry is, get magnesium oxide single crystal, metal oxide containing precious metals, rare earth oxide and water, grinding in ball grinder at least 6 hours, the addition of water was 300 ~ 500 times of the total amount of described magnesium oxide single crystal, metal oxide containing precious metals and rare earth oxide.
10. the preparation method of a kind of automobile three-way catalysts according to claim 6, is characterized in that: described acid solution is salpeter solution.
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| CN106867285A (en) * | 2017-01-21 | 2017-06-20 | 郑州人造金刚石及制品工程技术研究中心有限公司 | A kind of automobile three-way catalysts coating, the automobile three-way catalysts containing the coating and preparation method thereof |
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| CN106867285A (en) * | 2017-01-21 | 2017-06-20 | 郑州人造金刚石及制品工程技术研究中心有限公司 | A kind of automobile three-way catalysts coating, the automobile three-way catalysts containing the coating and preparation method thereof |
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