CN106492793B - A kind of electron beam irradiation modified material improves the active methods and applications of its catalytic denitration - Google Patents

A kind of electron beam irradiation modified material improves the active methods and applications of its catalytic denitration Download PDF

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CN106492793B
CN106492793B CN201610840385.1A CN201610840385A CN106492793B CN 106492793 B CN106492793 B CN 106492793B CN 201610840385 A CN201610840385 A CN 201610840385A CN 106492793 B CN106492793 B CN 106492793B
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CN106492793A (en
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马玲玲
罗敏
徐殿斗
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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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8628—Processes characterised by a specific catalyst
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    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44—Palladium
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
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    • B01D2251/202—Hydrogen
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

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Abstract

A kind of electron beam irradiation modified material improves the active methods and applications of its catalytic denitration, belongs to catalysis material technical field.Using aluminum titanium composite oxide as carrier, palladium is active constituent, and aluminum titanium composite oxide is prepared using sol-gel method, then gained catalyst after reduction is carried out radiation treatment by polyethylene glycol reduction method to get the catalyst of radiation modification by the addition of palladium.Its main feature is that radiation modification makes catalyst form flaky nanometer structure, it will be apparent that the temperature window for having widened catalysis reaction improves NO on palladium catalystxThe performance of removing.Preparation method simple process of the invention, easy to operate, modified catalyst has good denitration performance, has a good application prospect.

Description

A kind of electron beam irradiation modified material improves the active methods and applications of its catalytic denitration
Technical field
The present invention relates to a kind of Electron-beam Modified palladium catalyst and its preparation and using the catalyst under excess oxygen The method of Catalytic Decomposition of Nitric Oxide.Belong to catalysis material preparation and technical field of air pollution control.
Background technique
Nitrogen oxides is due to can result in the pollution problems such as acid rain, photochemical fog, NOxEmission control increasingly cause people Concern, wherein selective catalytic reduction (Selective Catalytic Reduction, SCR) is NO under excess oxygenx A kind of effective means of control.Use NH3When making reducing agent, the low temperature active (< 300 DEG C) of traditional vanadium tungsten titanium catalyst needs to be mentioned It is high；In addition, the toxicity of vanadium and leakage of ammonia etc. also limit NH3The application of-SCR.When hydrogen makees reducing agent, NOxIt can be By catalytic purification in the range of 100~300 DEG C, reduction temperature is substantially reduced, and excess hydrogen can generate water with oxygen combustion, Secondary pollution will not be generated.Therefore, hydrogen selective restores NOx(H2- SCR) become one of the effective means for removing NOx.
NOx is restored for hydrogen selective, common catalyst is noble metal catalyst, currently used H2- SCR catalysis Agent is mainly precious metals pd and Pt.In view of the price of Pd is low compared with Pt, the research of Pd base catalyst increasingly causes the pass of people Note.In order to reduce the production cost of catalyst, the content for reducing precious metals pd is significant to practical application.But your gold The low temperature active that the reduction of category load capacity will lead to Pd catalyst is decreased obviously.Therefore, the Pd of low-load amount and high activity is developed Based denitration catalyst, to reduce Air Pollutants NOx discharge, improve China air quality have great importance and Application prospect.
The present invention is by the electron beam irradiation modified palladium catalyst for being prepared for low-load amount, in relatively wide temperature model It encloses interior to NOxRemoving has good catalytic activity.
Summary of the invention
The object of the present invention is to provide a kind of preparation method, the low catalyst of simple and precious metals pd content, makes it to hydrogen Gas selective catalyst reduction of nitrogen oxides has good catalytic performance.Polyethylene glycol reduction method is as preparing nano-noble metal A kind of method, polyvinylpyrrolidone is added during the preparation process can control the nanoscale of noble metal, but existing ask Topic is that polyvinylpyrrolidone easily remains in the catalyst, to reduce the activity of catalyst.The present invention passes through electron beam irradiation It is modified, while effectively removing polyvinylpyrrolidone, so that catalyst is formed flaky nanometer structure, so that it is good to prepare performance Good Pd catalyst.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of modified palladium catalyst, which is characterized in that composition is expressed as Pd/TiO2-Al2O3, Pd is supported on TiO2-Al2O3 On (aluminum titanium composite oxide solid solution), wherein the mass percentage of Pd is 0.2-1.0%, TiO2And Al2O3Mass ratio be 2:8, modified palladium catalyst are flaky nanometer structure.And laminated structure stands on the plane at place.
The present invention provides a kind of electron beam irradiation modified materials to improve the active method of its catalytic denitration, i.e., a kind of electronics The preparation method of beam radiation modification palladium catalyst, it is characterised in that: this method successively the following steps are included:
(1) it is hydrolyzed at 80-90 DEG C aluminium isopropoxide 4-8 hours with deionized water, nitric acid is added to be allowed to form transparent colloidal sol, Then butyl titanate is added, so that the TiO generated2And Al2O3Mass ratio be 2:8, stir 6-10 hours, the gel of formation；
(2) then dry (to be done at preferably 120 DEG C by the aging (preferably aging for 24 hours) at room temperature of gel obtained by step (1) It is 10-12 hours dry), 4-8h finally is roasted at 450-600 DEG C in Muffle furnace, TiO is made2-Al2O3；
(3) step (2) resulting TiO is taken2-Al2O3In a certain amount of PdCl in reaction vessel, is added2Solution, polyethylene Pyrrolidones (PVP) and polyethylene glycol simultaneously mix, and are passed through N2Gas and circulating condensing water are protected, 160 DEG C is gradually heated to and heats Back flow reaction 4-8h；Centrifugation, filtering, filtration cakes torrefaction (preferably 80 DEG C drying 12-24 hours) will be taken out by liquid after reaction；
(4) the resulting solid of step (3) is subjected to electron beam irradiation, in the case where dosage rate is 20Gy/s-100Gy/s, irradiation Dosage is 10kGy~100kGy.
It is preferred that PdCl2: polyvinylpyrrolidone (PVP): polyethylene glycol molar ratio is 1:(10-30): (5-15), further It is preferred that 1:20:10.
The present invention also provides be used to remove NO using radiation modification palladium catalystxMethod, it is characterised in that the application Method the following steps are included:
(1) modified palladium catalyst is loaded in fixed bed reactors, reaction temperature is controlled in 100~300 DEG C of ranges；
(2) using hydrogen as reducing agent, control total gas flow rate in 150~300ml/min, air speed 52,000~104, 000h-1。
Compared with prior art, the present invention having the following advantages and outstanding effects: by electron beam irradiation, being catalyzed dosage form At flaky nanometer structure, and laminated structure stands on the plane (as shown in Figure 1) at place, the low temperature of the Pd catalyst of low-load amount Denitration activity significantly improves.Radiation modification makes catalyst form flaky nanometer structure, it will be apparent that has widened the temperature of catalysis reaction Window improves NO on palladium catalystxThe performance of removing.Preparation method simple process of the invention, easy to operate, Modified catalytic Agent has good denitration performance, has a good application prospect.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of catalyst non-irradiated (A) and 50kGy metering irradiation (B).
Specific embodiment
Typical technical solution of the invention is described further below with reference to embodiment, but the present invention is not limited to Following embodiment.
Embodiment 1:
0.5%Pd/TiO is irradiated under the conditions of dosage rate 50Gy/s, irradiation dose 10kGy2-Al2O3Catalyst preparation
A) it is hydrolyzed at 90 DEG C 16.02 grams of aluminium isopropoxides 4 hours with deionized water on a rotary evaporator, dust technology is added to make The transparent colloidal sol of formation, 8.52 grams of butyl titanates are then added, make TiO2And Al2O3Mass ratio be 2:8, stirring is 6 small When, the gel of formation；
B) by gel obtained by step a), aging is for 24 hours, 12 hours dry at 120 DEG C at room temperature, finally 500 in Muffle furnace 4h is roasted at DEG C, and TiO is made2-Al2O3；
C) the resulting TiO of step b) is taken2-Al2O3In in there-necked flask, the PdCl of 4.7ml 0.1mol/L is added2Solution, 9.4 ×10-3Mol polyvinylpyrrolidone (PVP) and 4.7 × 10-3Mol polyglycol solution simultaneously mixes, and is passed through N2Protect gas and circulation Condensed water is gradually heated to 160 DEG C and heating reflux reaction 4h.Liquid takes out centrifugation, filtering after reacting, and filter cake is dried at 80 DEG C It is 12 hours dry；
D) solid in step c) is taken to carry out electron beam irradiation, in the case where dosage rate is 50Gy, irradiation dose 10kGy, 10kGy is made and irradiates 0.5%Pd/TiO2-Al2O3Catalyst.
Embodiment 2:
0.5%Pd/TiO is irradiated under the conditions of dosage rate 50Gy/s, irradiation dose 50kGy2-Al2O3The preparation of catalyst
A) it is hydrolyzed at 90 DEG C 16.02 grams of aluminium isopropoxides 8 hours with deionized water on a rotary evaporator, dust technology is added to make The transparent colloidal sol of formation, 8.52 grams of butyl titanates are then added, make TiO2And Al2O3Mass ratio be 2:8, stirring is 10 small When, the gel of formation；
B) by gel obtained by step a), aging is for 24 hours, 10 hours dry at 120 DEG C at room temperature, finally 500 in Muffle furnace 4h is roasted at DEG C, and TiO is made2-Al2O3；
C) the resulting TiO of step b) is taken2-Al2O3In in there-necked flask, the PdCl of 4.7ml 0.1mol/L is added2Solution, 9.4 ×10-3Mol polyvinylpyrrolidone (PVP) and 4.7 × 10-3Mol polyglycol solution simultaneously mixes, and is passed through N2Protect gas and circulation Condensed water is gradually heated to 160 DEG C and heating reflux reaction 8h.Liquid takes out centrifugation, filtering after reacting, and filter cake is dried at 80 DEG C It is 24 hours dry；
D) solid in step c) is taken to carry out electron beam irradiation, in the case where dosage rate is 50Gy, irradiation dose 50kGy, 50kGy is made and irradiates 0.5%Pd/TiO2-Al2O3Catalyst.
Embodiment 3:
0.5%Pd/TiO is irradiated under the conditions of dosage rate 50Gy/s, irradiation dose 100kGy2-Al2O3The preparation of catalyst
A) it is hydrolyzed at 90 DEG C 16.02 grams of aluminium isopropoxides 4 hours with deionized water on a rotary evaporator, dust technology is added to make The transparent colloidal sol of formation, 8.52 grams of butyl titanates are then added, make TiO2And Al2O3Mass ratio be 2:8, stirring is 6 small When, the gel of formation；
B) by gel obtained by step a), aging is for 24 hours, 10 hours dry at 120 DEG C at room temperature, finally 450 in Muffle furnace 8h is roasted at DEG C, and TiO is made2-Al2O3；
C) the resulting TiO of step b) is taken2-Al2O3In in there-necked flask, the PdCl of 4.7ml 0.1mol/L is added2Solution, 9.4 ×10-3Mol polyvinylpyrrolidone (PVP) and 4.7 × 10-3Mol polyglycol solution simultaneously mixes, and is passed through N2Protect gas and circulation Condensed water is gradually heated to 160 DEG C and heating reflux reaction 4h.Liquid takes out centrifugation, filtering after reacting, and filter cake is dried at 80 DEG C It is 12 hours dry；
D) solid in step c) is taken to carry out electron beam irradiation, in the case where dosage rate is 50Gy, irradiation dose 100kGy, 100kGy is made and irradiates 0.5%Pd/TiO2-Al2O3Catalyst.
Comparative example 4:
Non-irradiated 0.5%Pd/TiO2-Al2O3The preparation of catalyst
A) it is hydrolyzed at 90 DEG C 16.02 grams of aluminium isopropoxides 4 hours with deionized water on a rotary evaporator, dust technology is added to make The transparent colloidal sol of formation, 8.52 grams of butyl titanates are then added, make TiO2And Al2O3Mass ratio be 2:8, stirring is 6 small When, the gel of formation；
B) by gel obtained by step a), aging is for 24 hours, 12 hours dry at 120 DEG C at room temperature, finally 500 in Muffle furnace 4h is roasted at DEG C, and TiO is made2-Al2O3；
C) the resulting TiO of step b) is taken2-Al2O3In in there-necked flask, the PdCl of 4.7ml 0.1mol/L is added2Solution, 9.4 ×10-3Mol polyvinylpyrrolidone (PVP) and 4.7 × 10-3Mol polyglycol solution simultaneously mixes, and is passed through N2Protect gas and circulation Condensed water is gradually heated to 160 DEG C and heating reflux reaction 4h.Liquid takes out centrifugation, filtering after reacting, and filter cake is dried at 80 DEG C It is 12 hours dry, up to non-irradiated 0.5%Pd/TiO2-Al2O3Catalyst.
Embodiment 5:
The preparation method of catalyst is same as Example 1, and 0.2g catalyst is loaded in fixed bed reactors, reaction Gas group becomes 0.25%NO, 1%H2, 5%O2, the flow velocity of reaction gas is 150ml/min, air speed 52,000h-1.Activity rating Temperature range is 100~300 DEG C, and under different temperatures, the conversion ratio of catalyst reduction nitrogen oxides is shown in Table 1.
Embodiment 6: the preparation method of catalyst is same as Example 2, and 0.2g catalyst is loaded in fixed bed reactors In the middle, reaction gas group becomes 0.25%NO, 1%H2, 5%O2, the flow velocity of reaction gas is 150ml/min, air speed 52,000h-1。 Activity rating temperature range is 100~300 DEG C, and under different temperatures, the conversion ratio of catalyst reduction nitrogen oxides is shown in Table 1.
Embodiment 7: the preparation method of catalyst is same as Example 3, and 0.2g catalyst is loaded in fixed bed reactors In the middle, reaction gas group becomes 0.25%NO, 1%H2, 5%O2, the flow velocity of reaction gas is 150ml/min, air speed 52,000h-1。 Activity rating temperature range is 100~300 DEG C, and under different temperatures, the conversion ratio of catalyst reduction nitrogen oxides is shown in Table 1.
Influence result of 1 radiation resistance of table to modified catalyst activity rating

Claims (8)

1. a kind of method that electron beam irradiation prepares modified palladium catalyst, it is characterised in that: modified palladium catalyst, composition are expressed as Pd/TiO2-Al2O3, Pd is supported on TiO2-Al2O3On, wherein the mass percentage of Pd is 0.2-1.0%, TiO2And Al2O3's Mass ratio is 2:8, and modified palladium catalyst is flaky nanometer structure；Method includes the following steps:
(1) it is hydrolyzed at 80-90 DEG C aluminium isopropoxide 4-8 hours with deionized water, adds nitric acid to be allowed to form transparent colloidal sol, then Butyl titanate is added, so that the TiO generated2And Al2O3Mass ratio be 2:8, stir 6-10 hours, the gel of formation；
(2) it by gel aging at room temperature obtained by step (1), then dries, finally roasts 4- at 450-600 DEG C in Muffle furnace TiO is made in 8h2-Al2O3；
(3) step (2) resulting TiO is taken2-Al2O3In a certain amount of PdCl in reaction vessel, is added2Solution, polyvinylpyrrolidine Ketone (PVP) and polyethylene glycol simultaneously mix, and are passed through N2Gas and circulating condensing water are protected, be gradually heated to 160 DEG C and is heated to reflux anti- Answer 4-8h；Liquid takes out centrifugation, filtering, filtration cakes torrefaction after reacting；
(4) the resulting solid of step (3) is subjected to electron beam irradiation, in the case where dosage rate is 20Gy/s-100Gy/s, irradiation dose For 10kGy~100kGy.
2. according to method of claim 1, which is characterized in that step (2) aging is for 24 hours, 10-12 hours dry at 120 DEG C.
3. according to method of claim 1, which is characterized in that PdCl2: polyvinylpyrrolidone (PVP): polyethylene glycol molar ratio For 1:(10-30): (5-15).
4. according to method of claim 1, which is characterized in that PdCl2: polyvinylpyrrolidone (PVP): polyethylene glycol molar ratio For 1:20:10.
5. according to method of claim 1, which is characterized in that step (3) it is dry for 80 DEG C drying 12-24 hours.
6. according to method of claim 1, which is characterized in that modified palladium catalyst, laminated structure stand on the plane at place.
7. the modification palladium catalyst being prepared according to method described in any one of claims 1-6.
8. the modification palladium catalyst being prepared according to method described in any one of claims 1-6 is for removing NOxMethod, It is characterized in that the application method the following steps are included:
(1) modified palladium catalyst is loaded in fixed bed reactors, reaction temperature is controlled in 100~300 DEG C of ranges；
(2) using hydrogen as reducing agent, control total gas flow rate is in 150~300ml/min, and air speed is 52,000~104,000h-1。
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