CN107899582A - Preparation method of monoblock type cobalt-base catalyst and products thereof and application - Google Patents
Preparation method of monoblock type cobalt-base catalyst and products thereof and application Download PDFInfo
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- CN107899582A CN107899582A CN201711099461.9A CN201711099461A CN107899582A CN 107899582 A CN107899582 A CN 107899582A CN 201711099461 A CN201711099461 A CN 201711099461A CN 107899582 A CN107899582 A CN 107899582A
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- 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
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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
- 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
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7022—Aliphatic hydrocarbons
Abstract
The invention discloses a kind of preparation method of monoblock type cobalt-base catalyst and products thereof and application, utilize electrochemical method, directly electro-deposition prepares catalyst in monoblock type foam nickel base, the load capacity of catalyst is adjusted by controlling sedimentation time, using cabaltous nitrate hexahydrate as raw material, after electrodeposited processing, then the nickel foam integral catalyzer material of Load Balanced can be obtained by roasting.This process simplify complicated traditional catalyst preparation mode.The advantages that present invention has raw material simple, and it is convenient to prepare, Load Balanced and stabilization, anti-sintering is particularly suitable for a small amount of of laboratory basic research and prepares.
Description
Technical field
The present invention relates to a kind of preparation method of monoblock type cobalt-base catalyst and products thereof and application, specifically with bubble
Foam nickel substrate directly utilizes the preparation method for being electrodeposited in supported on carriers cobalt-base catalyst as carrier.
Background technology
Current air pollution problem getting worse, using the VOC gas in catalyst oxidation air in terms of environmental protection
Have great importance.Compared with conventional particles type catalyst, integral catalyst bed layer specific surface area bigger, mass-transfer efficiency
The advantages that high, heat-resist, good mechanical property, therefore as the research hotspot in current environmental catalysis field.Integral catalyzer
The catalyst being made of skeleton matrix, scattered carrier, active component and four part of auxiliary agent is generally referred to, but due to catalyst material
The difference of material and preparation method, sharing carrier and auxiliary agent can selectively exist, and skeleton matrix and active component are then whole
Indispensable part in body formula catalyst.Skeleton carrier is the key factor for influencing integral catalyzer performance, is generally made pottery
Porcelain or metal_based material, possess ordered structure, and possess regular in a large amount of macro-scales or irregular hole.Carried in this two class
In body, metal_based material has physically better and mechanical property compared to ceramic based material, therefore more suitable for making catalyst
Carrier, and compared to traditional honeycomb carrier, it is unique that the metallic-based support of foam type has the advantages that：Matrix is close
Spend that small, specific surface area is big, three-dimensional structure is unique and the contact that can be obviously promoted between reactant and catalyst, so using foam
Base Metal carrier can more improve the catalytic capability of integral catalyzer.Foam metal as catalyst carrier has very
It is more, mainly there are foamed iron, nickel foam, foam copper etc..Wherein nickel foam is the most a kind of foam metal base carriers used.Remove
The selection of carrier, the preparation of catalyst and mode of loading are also an important factor for influencing integral catalyzer, to select letter
Easy row, reliable and stable mode of loading are extremely important.
It is to be impregnated or coated with the conventional method of supported on carriers catalyst activity component, but these methods have
Limitation.Both approaches are required for taking at present prepares catalyst in advance, and makes catalysis by the physical absorption ability of carrier
Agent is adhered to, and physical absorption is not a stable adhesive force.So although catalyst prepared by infusion process adheres to uniformly,
But adhesive force is smaller and unstable, and the amount of coating process supported catalyst is more but coating process controllability is not high, and is catalyzed
The load capacity of agent is unstable, also there is higher technical requirements to operator.A kind of so simple and practicable, convenient and reliable load side
Load of the method to integral catalyzer is extremely important, and although current infusion process and coating process cut both ways, but is loading
All there is certain limitation in terms of catalyst.
The content of the invention
Cumbersome for catalyst preparation in current technology and loading process takes, loads that uneven, adhesive force is less
Problems, present invention aims at：A kind of preparation method of monoblock type cobalt-base catalyst is provided.
Still a further object of the present invention is：A kind of monoblock type cobalt-base catalyst product is provided.
Another object of the present invention is：A kind of application of monoblock type cobalt-base catalyst is provided.
The present invention is achieved by the following technical solutions：A kind of preparation method of monoblock type cobalt-base catalyst, using six
Cobalt-base catalyst is directly prepared and is attached in foam nickel base, led to as raw material by nitric hydrate cobalt using electro-deposition method
Control sedimentation time is crossed to adjust the load capacity of catalyst, is comprised the following steps：
The first step, the small rectangle that width is 1cm is cut into by nickel foam volume；
Second step, weighs a certain amount of cabaltous nitrate hexahydrate and is dissolved in a certain amount of deionized water, stirs 10min；
3rd step, takes the prepared cobalt nitrate solutions of 40ml to be placed in a small beaker, and nickel foam small pieces are clipped in electrochemistry
On the working electrode of work station, by platinum electrode and calomel electrode connect respectively electrochemical workstation to electrode and reference electrode；
4th step, nickel foam small pieces, platinum electrode and calomel electrode are immersed in the small beaker equipped with cobalt nitrate solution at the same time, adjusted
Constant pressure electro-deposition program, sets deposition voltage -1V and correspondingly deposited time, starts to deposit；
5th step, removes the nickel foam small pieces for being loaded with active material after the completion of deposition, is placed in glass dish and is roused at 50 degree
In wind drying box, drying；
6th step, is positioned over Muffle kiln roasting, calcination temperature is 400 DEG C, roasting time 4h, heating by the carrier after drying
Speed is 2 DEG C/min.Up to monoblock type cobalt-based catalyst agent material.
Catalyst preparation, attachment integration, Load Balanced, adheres to stable integral catalyzer technology of preparing, using electricity
Cobalt-base catalyst can directly be prepared and is attached in foam nickel base by deposition process, quickly prepare a kind of the whole of Load Balanced
Body formula catalyst.Front and rear SEM characterizations are loaded and roasted by catalyst it can be found that catalyst Load Balanced in the present invention,
And pattern is excellent, catalyst morphology is stablized and does not change before and after roasting.The present invention only with cabaltous nitrate hexahydrate as raw material,
After electrodeposited processing, then the nickel foam integral catalyzer material of Load Balanced can be obtained by roasting.
Cobalt nitrate solution concentration in the second step is 0.1M, and concrete configuration is determined according to the amount of each deposited samples
The amount of solution.
The sedimentation time of 4th step is determined according to the amount of required catalyst activity material, selects 300s ~ 3600s.
A kind of monoblock type cobalt-base catalyst, it is characterised in that be prepared according to any of the above-described the method.
A kind of monoblock type cobalt-base catalyst is to C3H8Application in catalysis oxidation.
To ensure catalyst loads in experimentation uniformity and uniformity, each influence factor in deposition process should
Stringent control.The size of nickel foam substrate should be consistent, and the small beaker and amount of solution in deposition process should be also consistent,
Three electrodes in beaker should load effect in sustained height, because the efficiency highest that platinum electrode is deposited with working electrode when opposite
Fruit is best.This process simplify complicated traditional catalyst preparation mode,
The present invention has the following advantages：
（1）Catalyst is prepared using electro-deposition method, preparation process is simply controllable, it is not necessary to take additional time and prepare in advance
Catalyst.
（2）Prepare catalyst and supported catalyst synchronously carries out, by regarding the substrate of integral catalyzer as work electricity
Pole and directly in substrate growth catalyst.
（3）The catalyst Load Balanced of preparation, adhesive force is big, not easily to fall off, and pattern is good.
Brief description of the drawings
Fig. 1 is foam nickel base load C o3O4XRD diagram afterwards；
Fig. 2 is the SEM figures after embodiment 1 loads；
Fig. 3 is the Activity Results that Application Example obtains.
Embodiment
Elaborate below to the embodiment of the present invention：The present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
In the examples below, the size of foam nickel base has carried out cutting processing, the foam nickel sheet after handling
Width is 1cm, and the cabaltous nitrate hexahydrate solution configured is 1M.
Embodiment 1
The cabaltous nitrate hexahydrate solution for measuring 40mL 0.1M first is placed in 50 mL beakers.
Foam nickel sheet, platinum electrode, calomel electrode are sequentially connected the working electrode of upper electrochemical workstation, to electrode and ginseng
Compare electrode.Foam nickel sheet, platinum electrode, calomel electrode are positioned over the 50mL beakers equipped with 40mL cobalt nitrate solutions after connection
In, and three electrodes are kept in sustained height.Electrodeposition condition, deposition voltage -1V, sedimentation time 300s are set.
Material is dried into 1h in 50 DEG C of air dry ovens after the completion of deposition, 400 DEG C of roasting 4h in Muffle furnace is placed on, rises
Warm speed 2oC/min.Obtain uniform load Co3O4Foam nickel carrier integral catalyzer, loading is：3%.Fig. 1 is foam
Nickel substrate load C o3O4XRD diagram afterwards, Fig. 2 are the SEM figures after embodiment 1 loads.
Embodiment 2
The cabaltous nitrate hexahydrate solution for measuring 40mL 0.1M first is placed in 50 mL beakers.
Foam nickel sheet, platinum electrode, calomel electrode are sequentially connected the working electrode of upper electrochemical workstation, to electrode and ginseng
Compare electrode.Foam nickel sheet, platinum electrode, calomel electrode are positioned over the 50mL beakers equipped with 40mL cobalt nitrate solutions after connection
In, and three electrodes are kept in sustained height.Electrodeposition condition, deposition voltage -1V, sedimentation time 600s are set.
Material is dried into 1h in 50 DEG C of air dry ovens after the completion of deposition, 400 DEG C of roasting 4h in Muffle furnace is placed on, rises
Warm speed 2oC/min.Obtain uniform load Co3O4Foam nickel carrier integral catalyzer, loading is：4.5%.
Embodiment 3
The cabaltous nitrate hexahydrate solution for measuring 40mL 0.1M first is placed in 50 mL beakers.
Foam nickel sheet, platinum electrode, calomel electrode are sequentially connected the working electrode of upper electrochemical workstation, to electrode and ginseng
Compare electrode.Foam nickel sheet, platinum electrode, calomel electrode are positioned over the 50mL beakers equipped with 40mL cobalt nitrate solutions after connection
In, and three electrodes are kept in sustained height.Electrodeposition condition, deposition voltage -1V, sedimentation time 900s are set.
Material is dried into 1h in 50 DEG C of air dry ovens after the completion of deposition, 400 DEG C of roasting 4h in Muffle furnace is placed on, rises
Warm speed 2oC/min.Obtain uniform load Co3O4Foam nickel carrier integral catalyzer, loading is：6.5%
Embodiment 4
The cabaltous nitrate hexahydrate solution for measuring 40mL 0.1M first is placed in 50 mL beakers.
Foam nickel sheet, platinum electrode, calomel electrode are sequentially connected the working electrode of upper electrochemical workstation, to electrode and ginseng
Compare electrode.Foam nickel sheet, platinum electrode, calomel electrode are positioned over the 50mL beakers equipped with 40mL cobalt nitrate solutions after connection
In, and three electrodes are kept in sustained height.Electrodeposition condition, deposition voltage -1V, sedimentation time 1800s are set.
Material is dried into 1h in 50 DEG C of air dry ovens after the completion of deposition, 400 DEG C of roasting 4h in Muffle furnace is placed on, rises
Warm speed 2oC/min.Obtain uniform load Co3O4Foam nickel carrier integral catalyzer, loading is：11%
Embodiment 5
The cabaltous nitrate hexahydrate solution for measuring 40mL 0.1M first is placed in 50 mL beakers.
Foam nickel sheet, platinum electrode, calomel electrode are sequentially connected the working electrode of upper electrochemical workstation, to electrode and ginseng
Compare electrode.Foam nickel sheet, platinum electrode, calomel electrode are positioned over the 50mL beakers equipped with 40mL cobalt nitrate solutions after connection
In, and three electrodes are kept in sustained height.Electrodeposition condition, deposition voltage -1V, sedimentation time 3600s are set.
Material is dried into 1h in 50 DEG C of air dry ovens after the completion of deposition, 400 DEG C of roasting 4h in Muffle furnace is placed on, rises
Warm speed 2oC/min.Obtain uniform load Co3O4Foam nickel carrier integral catalyzer, loading is：16.5%
Application example
The Co of a 3600s deposition duration is prepared using above-mentioned electro-deposition method3O4Nickel foam base monolithic catalyst, and survey
It has been tried in the case where simulated atmosphere pollutes atmosphere to C3H8Catalytic activity, Fig. 3 is the Activity Results that Application Example obtains.Knot
Fruit shows, at 290 DEG C, loading is only 16.5% Co3O4Nickel foam base monolithic catalyst just can complete catalysts oxidation
C3H8Gas.
Claims (5)
1. a kind of preparation method of monoblock type cobalt-base catalyst, it is characterised in that using electro-deposition method that cobalt-base catalyst is straight
Connect and prepare and be attached in foam nickel base, adjust the load capacity of catalyst by controlling sedimentation time, comprise the following steps：
The first step, the small rectangle that width is 1cm is cut into by nickel foam volume；
Second step, weighs a certain amount of cabaltous nitrate hexahydrate and is dissolved in a certain amount of deionized water, stirs 10min；
3rd step, takes the prepared cobalt nitrate solutions of 40ml to be placed in a small beaker, and nickel foam small pieces are clipped in electrochemistry
On the working electrode of work station, by platinum electrode and calomel electrode connect respectively electrochemical workstation to electrode and reference electrode；
4th step, nickel foam small pieces, platinum electrode and calomel electrode are immersed in the small beaker equipped with cobalt nitrate solution at the same time, adjusted
Constant pressure electro-deposition program, sets deposition voltage -1V and correspondingly deposited time, starts to deposit；
5th step, removes the nickel foam small pieces for being loaded with active material after the completion of deposition, is placed in glass dish and is roused at 50 degree
In wind drying box, drying；
6th step, is positioned over Muffle kiln roasting, calcination temperature is 400 DEG C, roasting time 4h, heating by the carrier after drying
Speed is 2 DEG C/min.Up to monoblock type cobalt-based catalyst agent material.
2. the preparation method of monoblock type cobalt-base catalyst according to claim 1, it is characterised in that the nitre in the second step
Acidic cobalt solution concentration is 0.1M, and the amount of concrete configuration solution is determined according to the amount of each deposited samples.
3. the preparation method of monoblock type cobalt-base catalyst according to claim 1, it is characterised in that the deposition of the 4th step
Time determines according to the amount of required catalyst activity material, selects 300s ~ 3600s.
4. a kind of monoblock type cobalt-base catalyst, it is characterised in that be prepared according to any the methods of claim 1-3.
5. monoblock type cobalt-base catalyst is to C according to claim 43H8Application in catalysis oxidation.
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Cited By (7)
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| CN109433189A (en) * | 2018-12-17 | 2019-03-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of different valence state monoblock type manganese-based catalyst and products thereof and application |
| CN109569646A (en) * | 2018-12-23 | 2019-04-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of monoblock type cobalt manganese base binary catalyst and products thereof and application |
| JP2020028869A (en) * | 2018-08-24 | 2020-02-27 | 時空化学株式会社 | Method for producing voc removal catalyst, voc removal catalyst, and voc removal method |
| CN111203228A (en) * | 2020-03-05 | 2020-05-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Integral chromium oxide nitric oxide purifying catalyst and preparation method and application thereof |
| JP2020179327A (en) * | 2019-04-24 | 2020-11-05 | 時空化学株式会社 | Method for producing voc removal catalyst, voc removal catalyst, and voc removal method |
| CN113461140A (en) * | 2021-06-28 | 2021-10-01 | 烟台大学 | Cobalt-based molybdenum-manganese catalytic electrode and preparation method thereof |
| CN113529132A (en) * | 2021-08-09 | 2021-10-22 | 中国科学院海洋研究所 | Cobalt-based catalyst electrode and preparation method thereof |
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Cited By (11)
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| JP2020028869A (en) * | 2018-08-24 | 2020-02-27 | 時空化学株式会社 | Method for producing voc removal catalyst, voc removal catalyst, and voc removal method |
| JP7337338B2 (en) | 2018-08-24 | 2023-09-04 | 時空化学株式会社 | Method for producing catalyst for removing VOC and method for removing VOC |
| CN109433189A (en) * | 2018-12-17 | 2019-03-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of different valence state monoblock type manganese-based catalyst and products thereof and application |
| CN109569646A (en) * | 2018-12-23 | 2019-04-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of monoblock type cobalt manganese base binary catalyst and products thereof and application |
| JP2020179327A (en) * | 2019-04-24 | 2020-11-05 | 時空化学株式会社 | Method for producing voc removal catalyst, voc removal catalyst, and voc removal method |
| JP7344495B2 (en) | 2019-04-24 | 2023-09-14 | 時空化学株式会社 | Method for producing VOC removal catalyst, VOC removal catalyst and VOC removal method |
| CN111203228A (en) * | 2020-03-05 | 2020-05-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Integral chromium oxide nitric oxide purifying catalyst and preparation method and application thereof |
| CN111203228B (en) * | 2020-03-05 | 2022-04-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Integral chromium oxide nitric oxide purifying catalyst and preparation method and application thereof |
| CN113461140A (en) * | 2021-06-28 | 2021-10-01 | 烟台大学 | Cobalt-based molybdenum-manganese catalytic electrode and preparation method thereof |
| CN113461140B (en) * | 2021-06-28 | 2022-11-22 | 烟台大学 | Cobalt-based molybdenum-manganese catalytic electrode and preparation method thereof |
| CN113529132A (en) * | 2021-08-09 | 2021-10-22 | 中国科学院海洋研究所 | Cobalt-based catalyst electrode and preparation method thereof |
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Application publication date: 20180413 |