CN108499558A - Rb ionic compartmentation OMS-2 catalyst and its preparation method and application - Google Patents

Rb ionic compartmentation OMS-2 catalyst and its preparation method and application Download PDF

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CN108499558A
CN108499558A CN201810250990.2A CN201810250990A CN108499558A CN 108499558 A CN108499558 A CN 108499558A CN 201810250990 A CN201810250990 A CN 201810250990A CN 108499558 A CN108499558 A CN 108499558A
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oms
catalyst
acid
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rubidium
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侯静涛
董坤婷
李磊
沙振杰
汪明霞
谭文峰
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Huazhong Agricultural University
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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
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/32—Manganese, technetium or rhenium
    • B01J23/34—Manganese
    • 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
    • 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
    • B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • 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
    • B01D2257/00—Components to be removed
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    • B01D2257/7027—Aromatic hydrocarbons
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    • 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
    • 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
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/30—Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]

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Abstract

The invention discloses a kind of 2 catalyst of Rb ionic compartmentations OMS and its preparation method and application；The catalyst includes 2 carriers of OMS and active metal, and the active metal is Rb ions, and the Rb ion loads are in the duct of 2 carriers of the OMS；The molar ratio of the Rb ions and Mn in 2 carriers of the OMS are 0.001~0.5：1；Preparation method of the present invention is using potassium permanganate as oxidant, manganese nitrate reducing agent, and a certain concentration salting liquid containing Rb is introduced in system and has synthesized 2 catalyst of Rb ionic compartmentations OMS (Rb OMS 2) using a mild step hydrothermal synthesis method.Pass through the K in 2 molecular sieve pore passages of Rb ionic compartmentations OMS+This is tactful, and lattice oxygen activity is effectively promoted in 2 catalyst of OMS, to significantly promote catalytic purification VOCs activity.For this catalyst at 220~240 DEG C, benzene catalytic purification efficiency is more than 90%.

Description

Rb ionic compartmentation OMS-2 catalyst and its preparation method and application
Technical field
The present invention relates to catalyst technology, in particular to a kind of Rb ionic compartmentations OMS-2 catalyst and preparation method thereof and Using.
Background technology
Volatile organic matter (volatile organic compounds, VOCs) is common one of atmosphere pollution, It is mainly derived from the industries such as by-product, paint, the electronic chemical of petrochemical industry production, not only has significantly to human body Poisonous effect (such as irritation, teratogenesis, carcinogenic, mutagenesis), but also there is multiple environment effect (such as photochemistry cigarette Mist, destruction ozone layer, secondary organic aerosol etc.).In the past few decades, heat catalytic oxidation technology is due to having processing VOCs exhaust gas is efficient, without secondary pollution and the advantages that there is no adsorption saturations, is taken seriously.But at present use compared with Extensive catalyst is mainly the catalyst of carried noble metal (such as Pt, Pd), since the noble metals such as Pt and Pd are in the earth's crust Abundance only only has 3ppb and 0.6ppb, and resource is more in short supply, and economic cost is high, significantly limits it and is controlled in industrial VOCs Extensive use in reason.Therefore the catalyst developed cheap and easy to get, high activity and noble metal can be replaced to use, can not only Huge economic benefit is generated, and positive impetus will be played for the development of China's air pollution control technique.
Cryptomelane (KMn8O16, OMS-2) and it is by MnO6Octahedron connects to form 2 × 2 duct molecular sieves in the form of chain The Mn oxide of structure, due to its with cheap, environmental-friendly, unique physical and chemical performance such as：Pore structure, mixing Valence state (3+, 4+), be easy release Lattice Oxygen etc., it is considered to be most hopeful the catalytic purification for replacing noble metal for VOCs One of material, by people's extensive concern.But the low-temperature catalytic activity of unmodified OMS-2 is generally all very low, existing to pass through The means of metal substitution modification OMS-2 physical and chemical performances improve the low-temperature catalytic activity of OMS-2 to a certain extent, but Promotion amplitude is still very limited.Therefore, the catalytic activity that metal replaces OMS-2 how is further significantly promoted, will be Realize that substituting noble metal catalyst is applied to the key that VOCs is administered.
Invention content
Present invention aim to provide a kind of Rb ionic compartmentations OMS-2 catalyst and its preparation method and application, this Invention catalyst is cheap, catalytic purification VOCs is efficient, preparation process is simple.
To achieve the above object, the technical solution adopted by the present invention is：A kind of Rb ionic compartmentations OMS-2 catalyst, including OMS-2 carriers and active metal, the active metal are Rb ions, and the Rb ion loads are in the duct of the OMS-2 carriers It is interior；The molar ratio of the Rb ions and Mn in the OMS-2 carriers are 0.001~0.5：1.
Further, the Rb ion loads are in 2 × 2 molecular sieve pore passages of the OMS-2 carriers.
The preparation method of above-mentioned Rb ionic compartmentations OMS-2 catalyst, includes the following steps：
1) weigh that potassium permanganate is soluble in water, compound concentration is the liquor potassic permanganate of 0.0002~0.001mmol/mL；
2) Rb salt and acid are sequentially added into liquor potassic permanganate described in step 1), Rb salt presses Rb ions and potassium permanganate 0.001~0.1：0.02~0.1 molar ratio is added, and acid is 0.5~2.5 by with the liquor potassic permanganate volume ratio： 100 ratio is added, mixing；
3) manganese nitrate is added into step 2) acquired solution, manganese nitrate is pressed and potassium permanganate 0.01~0.05：0.02~ 0.1 molar ratio is added, mixing, the then reaction 12~for 24 hours in 60~90 DEG C of temperature and under confined conditions；
4) the Rb ionic compartmentations OMS-2 catalyst can be obtained after the washing of precipitate drying after reacting step 3).
Further, in the step 3), in Rb ions and the liquor potassic permanganate molar ratio of Mn be 0.001~ 0.5：1.
Further, in the step 2), acid is nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, hypochlorous acid, citric acid, acetic acid, hydrogen The mixing of one or more of fluoric acid, oxalic acid.
Further, in the step 2), Rb salt is rubidium nitrate, rubidium chloride, rubidium sulfate, rubidium acetate, rubidium fluoride RbF, carbonic acid The mixing of one or more of rubidium, rubidium iodide.
Further, in the step 4), drying temperature is 50~80 DEG C.
The application of above-mentioned Rb ionic compartmentations OMS-2 catalyst is urged using the Rb ionic compartmentations OMS-2 catalyst low temperature Change voloxidation organic matter, to reduce pollutant.
Further, using the Rb ionic compartmentations OMS-2 catalyst at 220~240 DEG C catalysis oxidation benzene.
Compared with prior art, the present invention has the following advantages：
One, catalyst of the present invention pass through this strategy of the K+ in Rb ionic compartmentation OMS-2 molecular sieve pore passages so that Lattice oxygen activity is effectively promoted in OMS-2 catalyst, improves the low-temperature catalytic activity of OMS-2, to significantly be promoted The activity of catalyst cleaning VOCs.The purification efficiency of catalyst of the present invention catalytic purification benzene at a temperature of 200~220 DEG C is super 50% is crossed, at 220~240 DEG C, the efficiency of catalytic purification benzene is more than 90%, and under equal conditions, activity, which is higher than, to undope The OMS-2 catalyst of Rb can sell Pt supported catalysts also superior to market.
Second, cheap Rb ions are successfully introduced into the duct of OMS-2 by the present invention so that this catalyst is honest and clean Valence is easy to get, high activity and as the catalyst that noble metal can be replaced to use, and solves the application warp of existing noble metal catalyst It helps of high cost, it is difficult to which the problems such as popularization and application produce huge economic and social benefits, are China's air pollution control technique Development play positive impetus.
Third, the present invention using potassium permanganate as oxidant, using manganese nitrate as reducing agent, introduces a certain concentration in system Salting liquid containing Rb has synthesized Rb ionic compartmentation OMS-2 catalyst (Rb-OMS-2), work using a mild step hydrothermal synthesis method The simple smooth, simple operation of skill flow further reduced production cost.
Description of the drawings
Fig. 1 is the distinctive X-ray diffraction figure (XRD) of Rb ionic compartmentation OMS-2 catalyst.
Fig. 2 is the CO adsorption process heating figure (CO-TPR) of Rb ionic compartmentation OMS-2 catalyst.
Fig. 3 is the activity figure of Rb ionic compartmentation OMS-2 catalyst Oxybenzenes.
Fig. 4 is Rb ionic compartmentation OMS-2 catalyst stability diagrams.
Specific implementation mode
With reference to specific embodiment, the present invention is described in further detail, convenient for more clearly understanding the present invention, But they do not constitute the present invention and limit.
Embodiment 1
(1) potassium permanganate for weighing 0.02mmol is dissolved in the distilled water of 100mL, is dissolved under magnetic stirring apparatus；
(2) by the rubidium nitrate of 0.001mmol, (the Rb salt can be rubidium nitrate, rubidium chloride, rubidium sulfate, rubidium acetate, fluorination The mixing of one or more of rubidium, rubidium carbonate, rubidium iodide) and 0.5mL sulfuric acid (acid can be nitric acid, hydrochloric acid, sulfuric acid, The mixing of one or more of phosphoric acid, hypochlorous acid, citric acid, acetic acid, hydrofluoric acid, oxalic acid) it is successively added in step (1) Solution, mixing；
(3) manganese nitrate of 0.01mmol is added in step (2) solution, then mixing seals beaker with preservative film Mouthful, it is reacted for 24 hours at 70 DEG C.
(4) to the end of reaction, it is 100 μ s/cm that above-mentioned substrate obtained by the reaction, which is washed with distilled water to conductivity,；It will Sample after washing is placed dries at 50 DEG C, you can to obtain 0.033Rb-OMS-2 catalyst.
Catalyst Discriminating materials：The XRD spectrum for the catalyst that embodiment 1 obtains is as shown in Figure 1, be cryptomelane structure.
The lattice oxygen activity of catalyst：The catalyst CO temperature programmed reductions peak peak that embodiment 1 is prepared, first Peak is happened at 215 DEG C, and 226 DEG C of the temperature of the reduction peak less than OMS-2 illustrates, higher in low temperature lattice oxygen activity.
Catalyst activity is evaluated：A concentration of 2000mg/m of benzene3, air speed 48000h-1, the conversion of gas chromatographic detection benzene Rate and CO2Production rate.The sample prepared using embodiment 1 is catalyst, the T of catalyzing, oxidizing and purifying benzene50And T90(the catalysis of benzene Oxidation, purification rate is respectively the temperature corresponding to 50% and 90%) it is respectively 195 DEG C and 218 DEG C (Fig. 2), as shown in figure 3, real Applying the purification efficiency of the low-temperature catalytic oxidation benzene of the catalyst of the gained of example 1, to be better than certain commodity Pt sold market under equal conditions negative Carried catalyst (T50=204 DEG C, T90=260 DEG C).
Catalyst stability is evaluated：As shown in figure 4, the rubidium ion prepared by embodiment 1 replaces OMS-2 catalyst in benzene A concentration of 2000mg/m3, air speed 48000h-1When, the catalytic conversion of continuous work 48h, benzene still remain in 96% or more, With good stability.
Embodiment 2
(1) potassium permanganate for weighing 0.02mmol is dissolved in the distilled water of 100mL, is dissolved under magnetic stirring apparatus；
(2) sulfuric acid of the rubidium nitrate of 0.003mmol and 0.5mL are successively added to solution in step (1), mixing；
(3) manganese nitrate of 0.01mmol is added in step (2) solution, then mixing seals beaker with preservative film Mouthful, it is reacted for 24 hours at 70 DEG C.
(4) to the end of reaction, it is 100 μ s/cm that above-mentioned substrate obtained by the reaction, which is washed with distilled water to conductivity,；It will Sample after washing is placed dries at 50 DEG C, you can to obtain 0.1Rb-OMS-2 catalyst.
Catalyst Discriminating materials：The XRD spectrum for the catalyst that embodiment 2 obtains is as shown in Figure 1, be cryptomelane structure.
Catalyst activity is evaluated：A concentration of 2000mg/m of benzene3, air speed 48000h-1, the conversion of gas chromatographic detection benzene Rate and CO2Production rate.The sample prepared using embodiment 2 is catalyst, the T of catalyzing, oxidizing and purifying benzene50And T90(the catalysis of benzene Oxidation, purification rate is respectively the temperature corresponding to 50% and 90%) it is respectively 211 DEG C and 239 DEG C (Fig. 3), as shown in figure 3, real Apply the T of the low-temperature catalytic oxidation benzene of the catalyst of 2 gained of example90Purification efficiency is better than certain commodity Pt sold market under equal conditions Supported catalyst (T50=204 DEG C, T90=260 DEG C).
Embodiment 3
(1) potassium permanganate for weighing 0.02mmol is dissolved in the distilled water of 100mL, is dissolved under magnetic stirring apparatus；
(2) sulfuric acid of the rubidium nitrate of 0.006mmol and 0.5mL are successively added to solution in step (1), mixing；
(3) manganese nitrate of 0.01mmol is added in step (2) solution, then mixing seals beaker with preservative film Mouthful, it is reacted for 24 hours at 70 DEG C.
(4) to the end of reaction, it is 100 μ s/cm that above-mentioned substrate obtained by the reaction, which is washed with distilled water to conductivity,；It will Sample after washing is placed dries at 50 DEG C, you can to obtain 0.3Rb-OMS-2 catalyst.
Catalyst Discriminating materials：The XRD spectrum for the catalyst that embodiment 3 obtains is as shown in Figure 1, be cryptomelane structure.
Catalyst activity is evaluated：A concentration of 2000mg/m of benzene3, air speed 48000h-1, the conversion of gas chromatographic detection benzene Rate and CO2Production rate.The sample prepared using embodiment 3 is catalyst, the T of catalyzing, oxidizing and purifying benzene50And T90(the catalysis of benzene Oxidation, purification rate is respectively the temperature corresponding to 50% and 90%) it is respectively 203 DEG C and 229 DEG C (Fig. 3), as shown in figure 3, real Apply the T of the low-temperature catalytic oxidation benzene of the catalyst of 3 gained of example90Purification efficiency is better than certain commodity Pt sold market under equal conditions Supported catalyst (T50=204 DEG C, T90=260 DEG C).

Claims (9)

1. a kind of Rb ionic compartmentations OMS-2 catalyst, including OMS-2 carriers and active metal, it is characterised in that：The activity gold It is Rb ions to belong to, and the Rb ion loads are in the duct of the OMS-2 carriers；In the Rb ions and the OMS-2 carriers The molar ratio of Mn is 0.001~0.5：1.
2. Rb ionic compartmentations OMS-2 catalyst according to claim 1, it is characterised in that：The Rb ion loads are described In 2 × 2 molecular sieve pore passages of OMS-2 carriers.
3. the preparation method of Rb ionic compartmentations OMS-2 catalyst, includes the following steps described in claim 1：
1) weigh that potassium permanganate is soluble in water, compound concentration is the liquor potassic permanganate of 0.0002~0.001mmol/mL；
2) Rb salt and acid are sequentially added into liquor potassic permanganate described in step 1), Rb salt is by Rb ions and potassium permanganate 0.001 ~0.1：0.02~0.1 molar ratio is added, and acid is 0.5~2.5 by with the liquor potassic permanganate volume ratio：100 ratio Example is added, mixing；
3) manganese nitrate is added into step 2) acquired solution, manganese nitrate is pressed and potassium permanganate 0.01~0.05：0.02~0.1 rubs Your ratio is added, mixing, the then reaction 12~for 24 hours in 60~90 DEG C of temperature and under confined conditions；
4) the Rb ionic compartmentations OMS-2 catalyst can be obtained after the washing of precipitate drying after reacting step 3).
4. the preparation method of Rb ionic compartmentations OMS-2 catalyst according to claim 3, it is characterised in that：The step 3) In, the molar ratio of Rb ions and Mn in the liquor potassic permanganate are 0.001~0.5：1.
5. according to the preparation method of the Rb ionic compartmentations OMS-2 catalyst of claim 3 or 4, it is characterised in that：The step 2) in, acid is the mixed of one or more of nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, hypochlorous acid, citric acid, acetic acid, hydrofluoric acid, oxalic acid It closes.
6. according to the preparation method of the Rb ionic compartmentations OMS-2 catalyst of claim 3 or 4, it is characterised in that：The step 2) in, Rb salt is the mixed of one or more of rubidium nitrate, rubidium chloride, rubidium sulfate, rubidium acetate, rubidium fluoride RbF, rubidium carbonate, rubidium iodide It closes.
7. according to the preparation method of the Rb ionic compartmentations OMS-2 catalyst of claim 3 or 4, it is characterised in that：The step 4) in, drying temperature is 50~80 DEG C.
8. the application of Rb ionic compartmentations OMS-2 catalyst according to claim 1, it is characterised in that：Utilize the Rb ions Replace OMS-2 catalyst low-temperature catalytic oxidation volatile organic matters, to reduce pollutant.
9. the application of Rb ionic compartmentations OMS-2 catalyst according to claim 8, it is characterised in that：Utilize the Rb ions Replace OMS-2 catalyst catalysis oxidation benzene at 220~240 DEG C.
CN201810250990.2A 2018-03-26 2018-03-26 Rb ionic compartmentation OMS-2 catalyst and its preparation method and application Pending CN108499558A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109364912A (en) * 2018-09-29 2019-02-22 华中农业大学 Alkaline-earth metal ions replace OMS-2 catalyst and its preparation method and application

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109364912A (en) * 2018-09-29 2019-02-22 华中农业大学 Alkaline-earth metal ions replace OMS-2 catalyst and its preparation method and application

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