CN106268915A - Minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material and synthesis technique thereof and application - Google Patents
Minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material and synthesis technique thereof and application Download PDFInfo
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- CN106268915A CN106268915A CN201610560259.0A CN201610560259A CN106268915A CN 106268915 A CN106268915 A CN 106268915A CN 201610560259 A CN201610560259 A CN 201610560259A CN 106268915 A CN106268915 A CN 106268915A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/041—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41
- B01J29/042—Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41 containing iron group metals, noble metals or copper
- B01J29/044—Iron group metals or copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0316—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing iron group metals, noble metals or copper
- B01J29/0333—Iron group metals or copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
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Abstract
The invention discloses minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material and synthesis technique thereof and application, the process of synthesis technique: template, dehydrated alcohol, brium carbonate, magnesium nitrate mix and blend are prepared barium magnesium complex solution；The stirring of cerous nitrate, dehydrated alcohol, zirconium nitrate, ferric nitrate prepares cerium ferrozirconium composite solution, and obtains cerium ferrozirconium barium magnesium complex solution with barium magnesium complex solution mix and blend；Palladous chloride., dehydrated alcohol, chloroplatinic acid, radium chloride mix and blend obtain palladium platinum rhodium composite solution；Palladium platinum rhodium composite solution is instilled in cerium ferrozirconium barium magnesium complex solution after stirring quantitatively vacuum metallizing, on carrier, is dried 3 hours for 40 DEG C 60 DEG C, 400 DEG C of 600 DEG C of roastings 6 hours and get final product.The present invention uses vac sorb plating roasting method, only needs plating 1 time, and technique is simple, and cost ratio is low, keeps high-performance, and service life is long, makes vehicle exhaust can reach discharge standard, and energy saving economy environmental protection.
Description
Technical field
The present invention relates to vent gas treatment field of material technology, specifically minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material
And synthesis technique and application.
Background technology
The dynamics that at present Environmental is administered is increasing, to the management of industrial waste gas and motor vehicle exhaust emission increasingly
Strictly, along with the issue of gasoline motor car exhausted gas state five standard, traditional automobile three unique catalytic converter can not be fully achieved
Emission request, and the production cost of automobile three-way catalyst is more and more higher, easily causes environmental pollution in production process.Currently used
Three-element catalytic agent producing process be the viscous glutinous roasting method of vac sorb, need vac sorb viscous glutinous 2-4 time.Complex process is loaded down with trivial details, becomes
This height, easily causes environmental pollution in production process, and when using on automobile, by the high flow rate of vehicle exhaust, high-temperature, height
Moisture, the impact of high concussion, easily cause the working substance on three-way catalyst and come off loss, thus affect the property of three-way catalyst
Energy and service life.
Summary of the invention
It is an object of the invention to provide and keep high-performance, length in service life, the minute amount of noble metal of energy saving economy environmental protection to change
Property cerium zirconium meso-porous molecular sieve material and synthesis technique and application, with the problem solving to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
The synthesis technique of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material, comprises the following steps:
1) claim 30-40g template to be dissolved in 200g dehydrated alcohol, add 5-10g brium carbonate, 10-20g magnesium nitrate, stirring
2.5-3.5 hour, prepare barium magnesium complex solution；
2) claim 20-60g cerous nitrate to be dissolved in 200g dehydrated alcohol, add 10-50g zirconium nitrate, add 20-30g ferric nitrate
Stir 2 hours, prepare cerium ferrozirconium composite solution；
3) prepared cerium ferrozirconium composite solution is added dropwise in barium magnesium complex solution uniformly, stirs 3.5-4.5 hour,
Synthesis prepares cerium ferrozirconium barium magnesium complex solution；
4) claim 0.2-2g Palladous chloride. to be dissolved in 200g dehydrated alcohol, add 0.1-0.5g chloroplatinic acid, 0.3-1g radium chloride, stir
Mix 1.5-2.5 hour, prepare palladium platinum rhodium composite solution；
5) palladium platinum rhodium composite solution is added dropwise to uniformly in cerium ferrozirconium barium magnesium complex solution, stirs 3.5-4.5 hour,
Synthesis minute amount of noble metal modification cerium zirconium mesopore molecular sieve solution；
6) by the minute amount of noble metal modification cerium zirconium quantitative vacuum metallizing of mesopore molecular sieve solution of synthesis on carrier, 40 DEG C-
Dry 3 hours for 60 DEG C, 400 DEG C of-600 DEG C of roastings 6 hours, prepare minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material.
As the further scheme of the present invention: carrier is gold violet stone ceramic honey comb.
As the further scheme of the present invention: step 1) in, claim 35g template to be dissolved in 200g dehydrated alcohol, mixing time
It it is 3 hours.
As the further scheme of the present invention: step 2) in, mixing time is 2 hours.
As the further scheme of the present invention: step 3) in, mixing time is 4 hours.
As the further scheme of the present invention: step 4) in, mixing time is 2 hours.
As the further scheme of the present invention: step 5) in, mixing time is 4 hours.
It is a further object of the present invention to provide the minute amount of noble metal modification cerium zirconium mesopore molecular sieve that above-mentioned synthesis technique prepares
Material.
It is yet another object of the invention to provide described minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material in automobile ternary
Application on catalyst.
Compared with prior art, the invention has the beneficial effects as follows:
The synthesis technique that the present invention provides is vac sorb plating roasting method, only needs plating 1 time.Technique is simple, cost ratio
Currently used three-way catalyst is low, and working substance after roasting, makes working substance melt with carrier through vac sorb plating on carrier
Be integrated, not by vehicle exhaust high flow rate, high-temperature, high-moisture, height shakes is affected, and keeps high-performance, service life is long.
Minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material is applied on automobile three-way catalyst, can reach discharge standard, and energy-conservation
Economic and environment-friendly.
Accompanying drawing explanation
Fig. 1 is the artwork synthesizing E liquid in the embodiment of the present invention；
Fig. 2 is the artwork that E liquid makes minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, all
Belong to the scope of protection of the invention.
Embodiment 1
Refer to Fig. 1-2, in the embodiment of the present invention, the synthesis work of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material
Skill, comprises the following steps:
1) claim 30g template to be dissolved in 200g dehydrated alcohol, add 5g brium carbonate, 10g magnesium nitrate, stir 3 hours, prepare barium
Magnesium complex solution is stand-by, is designated as A liquid.
2) claim 20g cerous nitrate to be dissolved in 200g dehydrated alcohol, add 10g zirconium nitrate, add 20g ferric nitrate and stir 2 hours,
Prepare cerium ferrozirconium composite solution, be designated as B liquid.
3) being added dropwise to uniformly in A liquid by prepared B liquid, stir 4 hours, it is molten that synthesis prepares cerium ferrozirconium barium magnesium complex
Liquid, is designated as C liquid.
4) claim 0.2g Palladous chloride. to be dissolved in 200g dehydrated alcohol, add 0.1g chloroplatinic acid, 0.3g radium chloride, stir 2 hours,
Prepare palladium platinum rhodium composite solution, be designated as D liquid.
5) being added dropwise to uniformly in C liquid by D liquid, stir 4 hours, synthesis minute amount of noble metal modification cerium zirconium mesopore molecular sieve is molten
Liquid, is designated as E liquid.
6) by the quantitative vacuum metallizing of E liquid of synthesis on carrier, dry 3 hours for 40 DEG C, 400 DEG C of roastings 6 hours, prepare micro-
Amount modified with noble metals cerium zirconium meso-porous molecular sieve material.
Embodiment 2
Refer to Fig. 1-2, in the embodiment of the present invention, the synthesis work of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material
Skill, comprises the following steps:
1) claim 40g template to be dissolved in 200g dehydrated alcohol, add 10g brium carbonate, 20g magnesium nitrate, stir 3 hours, prepare
Barium magnesium complex solution is stand-by, is designated as A liquid.
2) claim 60g cerous nitrate to be dissolved in 200g dehydrated alcohol, add 50g zirconium nitrate, add 30g ferric nitrate and stir 2 hours,
Prepare cerium ferrozirconium composite solution, be designated as B liquid.
3) being added dropwise to uniformly in A liquid by prepared B liquid, stir 4 hours, it is molten that synthesis prepares cerium ferrozirconium barium magnesium complex
Liquid, is designated as C liquid.
4) claim 2g Palladous chloride. to be dissolved in 200g dehydrated alcohol, add 0.5g chloroplatinic acid, 1g radium chloride, stir 2 hours, prepare
Palladium platinum rhodium composite solution, is designated as D liquid.
5) being added dropwise to uniformly in C liquid by D liquid, stir 4 hours, synthesis minute amount of noble metal modification cerium zirconium mesopore molecular sieve is molten
Liquid, is designated as E liquid.
6) by the quantitative vacuum metallizing of E liquid of synthesis on carrier, dry 3 hours for 60 DEG C, 600 DEG C of roastings 6 hours, prepare micro-
Amount modified with noble metals cerium zirconium meso-porous molecular sieve material.
Embodiment 3
Refer to Fig. 1-2, in the embodiment of the present invention, the synthesis work of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material
Skill, comprises the following steps:
1) claim 35g template to be dissolved in 200g dehydrated alcohol, add 8g brium carbonate, 15g magnesium nitrate, stir 3 hours, prepare barium
Magnesium complex solution is stand-by, is designated as A liquid.
2) claim 40g cerous nitrate to be dissolved in 200g dehydrated alcohol, add 30g zirconium nitrate, add 25g ferric nitrate and stir 2 hours,
Prepare cerium ferrozirconium composite solution, be designated as B liquid.
3) being added dropwise to uniformly in A liquid by prepared B liquid, stir 4 hours, it is molten that synthesis prepares cerium ferrozirconium barium magnesium complex
Liquid, is designated as C liquid.
4) claim 1g Palladous chloride. to be dissolved in 200g dehydrated alcohol, add 0.3g chloroplatinic acid, 0.7g radium chloride, stir 2 hours, system
Obtain palladium platinum rhodium composite solution, be designated as D liquid.
5) being added dropwise to uniformly in C liquid by D liquid, stir 4 hours, synthesis minute amount of noble metal modification cerium zirconium mesopore molecular sieve is molten
Liquid, is designated as E liquid.
6) by the quantitative vacuum metallizing of E liquid of synthesis on carrier, dry 3 hours for 50 DEG C, 500 DEG C of roastings 6 hours, prepare micro-
Amount modified with noble metals cerium zirconium meso-porous molecular sieve material.
Prospect analysis of market
The domestic market demand conservative estimation about 24,000,000 liters to gasoline car three-way catalyst, along with tail-gas from gasoline automobiles
The issue of discharge state five standard, the production cost of conventional gasoline car three-way catalyst necessarily improves, and can not be fully achieved discharge
Standard, so only carrying out technological innovation, selects new material and new technology to solve this difficult problem, and this is just to our trace
Modified with noble metals cerium zirconium meso-porous molecular sieve material application opportunity.By the quantitative vacuum metallizing of E liquid of synthesis at gold violet stone ceramic honey comb
On carrier, drying 3 hours for 40 DEG C, 400 DEG C of-600 DEG C of roastings 6 hours, (i.e. minute amount of noble metal changes to prepare gasoline engine three-way catalyst
Property cerium zirconium meso-porous molecular sieve material).The uniform plating of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material is at gold violet after testing
On stone honeycomb ceramic carrier, combine together with carrier, and performance is splendid.1, gasoline motor car exhausted gas state five standard can be reached.2、
The production technology making automobile three-way catalyst simplifies, and improves production capacity.3, the life of gasoline car three-way catalyst manufacturer can be made
Produce cost and reduce 30%-40%, 4, production process energy-conserving and environment-protective.In sum, minute amount of noble metal modification cerium zirconium mesopore molecular sieve
Material having a extensive future on automobile three-way catalyst.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter
From the point of view of which point, all should regard embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all by fall in the implication of equivalency and scope of claim
Change is included in the present invention.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only wraps
Containing an independent technical scheme, this narrating mode of description is only that for clarity sake those skilled in the art should
Description can also be formed those skilled in the art through appropriately combined as an entirety, the technical scheme in each embodiment
May be appreciated other embodiments.
Claims (9)
1. the synthesis technique of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material, it is characterised in that comprise the following steps:
1) claim 30-40g template to be dissolved in 200g dehydrated alcohol, add 5-10g brium carbonate, 10-20g magnesium nitrate, stir 2.5-3.5
Hour, prepare barium magnesium complex solution；
2) claim 20-60g cerous nitrate to be dissolved in 200g dehydrated alcohol, add 10-50g zirconium nitrate, add 20-30g ferric nitrate stirring 2
Hour, prepare cerium ferrozirconium composite solution；
3) prepared cerium ferrozirconium composite solution is added dropwise in barium magnesium complex solution uniformly, stirs 3.5-4.5 hour, synthesis
Prepare cerium ferrozirconium barium magnesium complex solution；
4) claim 0.2-2g Palladous chloride. to be dissolved in 200g dehydrated alcohol, add 0.1-0.5g chloroplatinic acid, 0.3-1g radium chloride, stirring
1.5-2.5 hour, prepare palladium platinum rhodium composite solution；
5) palladium platinum rhodium composite solution is added dropwise to uniformly in cerium ferrozirconium barium magnesium complex solution, stirs 3.5-4.5 hour, synthesis
Minute amount of noble metal modification cerium zirconium mesopore molecular sieve solution；
6) by the minute amount of noble metal modification cerium zirconium quantitative vacuum metallizing of mesopore molecular sieve solution of synthesis on carrier, 40 DEG C-60 DEG C
Dry 3 hours, 400 DEG C of-600 DEG C of roastings 6 hours, prepare minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material.
The synthesis technique of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material the most according to claim 1, its feature exists
In, carrier is gold violet stone ceramic honey comb.
The synthesis technique of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material the most according to claim 1, its feature exists
In, step 1) in, claim 35g template to be dissolved in 200g dehydrated alcohol, mixing time is 3 hours.
The synthesis technique of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material the most according to claim 1, its feature exists
In, step 2) in, mixing time is 2 hours.
The synthesis technique of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material the most according to claim 1, its feature exists
In, step 3) in, mixing time is 4 hours.
The synthesis technique of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material the most according to claim 1, its feature exists
In, step 4) in, mixing time is 2 hours.
The synthesis technique of minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material the most according to claim 1, its feature exists
In, step 5) in, mixing time is 4 hours.
8. the minute amount of noble metal modification cerium zirconium mesopore molecular sieve material prepared according to the arbitrary described synthesis technique of claim 1-7
Material.
Minute amount of noble metal modification cerium zirconium meso-porous molecular sieve material the most according to claim 8 is on automobile three-way catalyst
Application.
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