CN104841442A - Preparation method of anti-carbon deposition mesoporous confinement methane dry reforming catalyst - Google Patents
Preparation method of anti-carbon deposition mesoporous confinement methane dry reforming catalyst Download PDFInfo
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Abstract
The invention discloses a preparation method of an anti-carbon deposition mesoporous confinement highly-dispersed nickel-based methane dry reforming catalyst. According to the anti-carbon deposition mesoporous confinement highly-dispersed nickel-based methane dry reforming catalyst, a refractory oxide with ordered mesopore passages is taken as a carrier, and high dispersion of nickel in the passages is realized. According to the preparation method, a mesoporous oxide wit high temperature stability is taken as a reactant; a nickel precursor salt is delivered into the mesopore passages by alcohol; the inner surface of the mesopore passages are modified with alcoholic hydroxyl groups, so that nickel is dispersed preferably; and the methane dry reforming catalyst with excellent carbon deposition resistance and sintering resistance, and high activity and stability is obtained via vacuum drying, high-temperature calcinations, and H2-TPR (hydrogen temperature-programmed desorption) reduction. The preparation method is simple; cost is low; no environment pollution is caused; and catalytic efficiency is high.
Description
Technical field
The present invention relates to the preparation method of the dry reforming catalyst of a kind of anti-carbon mesoporous confinement methane, belong to nanocatalyst preparation technology and environmental protection technical field.
Background technology
Along with petroleum resources are day by day exhausted and environmental pollution day by day serious, development and utilization is cleaned, the fuel source of cheapness is subject to the common concern of various countries.Natural gas is fuel the cleanest at present, and it has pollutes little feature, is optimal chemical industry raw material.Nature is richly stored with natural gas resource, and natural gas (methane) is the chemical fuel resource enriched very much.From the trend of world energy sources development, the ratio of natural gas in energy resource structure will grow steadily.In recent years, strengthened just gradually in the status of gas chemical industry in industrial production and national economy.The chemical utilization of natural gas can be divided into directly conversion and indirect reformer two kinds of Basic Ways.The direct translation method of natural gas comprises the direct synthesis of methyl alcohol and formaldehyde, the preparation of HCN, the synthesis of aromatic hydrocarbons, methane oxidation coupling etc.Indirect reformer method is first synthesis gas methane conversion, further synthetic ammonia, methyl alcohol, or utilize CO to synthesize a series of fine chemical product and fuel and alkene again, and this is right most widely used technology path in gasification work at present.In natural gas indirect reformer utilization ways, basis and the tap of methane conversion to be synthesis gas be whole gas chemical industry.Traditional process for methane conversion comprises steam transforming method, partial oxidation process and carbon dioxide conversion method.
The whole catalyst of methane dry weight is mainly divided into noble metal catalyst (Ru, Pd, Pt etc.) and non-precious metal catalyst (Fe, Co, Ni etc.), noble metal catalyst has good anti-carbon, but due to expensive, resource scarcity, and noble metal active component can sinter loss under the high temperature conditions, so be necessary very much to study non-precious metal catalyst.Catalytic activity with nickel in base metal is best, and therefore we mainly study nickel-base catalyst to carry out methane reforming reaction.But nickel-base catalyst exists a fatal shortcoming, under long pyroreaction, the easy carbon distribution of nickel-base catalyst and metallic nickel sintering, thus cause catalysqt deactivation.Theoretical research proves: only have nickel size to a certain extent little, just may suppress the coring and increment of carbon fiber, thus reach anti-carbon object.Usually by interaction active constituent loading to carrier come between reinforcement metal carrier to improve catalytic stability and the anti-carbon anti-sintering property of catalyst.Recently, Ni, by the confinement effect in carrier duct, is fixed therein thus reaches good anti-sintering and anti-carbon effect by numerous research.But nickel nano particle is difficult to be transported in the mesopore orbit of carrier, major part is still attached to the outer surface of mesopore orbit, therefore well can't play anti-sintering and anti-carbon effect.
Summary of the invention
The present invention relates to the preparation method of the dry reforming catalyst of a kind of anti-carbon mesoporous confinement methane, belong to nanocatalyst preparation technology and environmental protection technical field.The nickel particle that in this catalyst, size is little and homogeneous is fine must be dispersed in the mesopore orbit of refractory oxide support, and duct wall energy plays the effect of confinement, therefore effectively can must inhibit growing up of metallic nickel nano granule.By the interpolation of Ce, reducing soot level further, is that in methane reforming, a kind of catalytic performance is good, and the simple nanocatalyst of preparation process.
Method for preparing catalyst of the present invention, comprises following steps:
Take appropriate cerium precursor salt and mesopore oxide is dissolved in deionized water, the load capacity of cerium is 3wt% ~ 5wt%, mix and blend 7 ~ 8h, dries to obtain the mesopore oxide carrier modified of Ce.The mesopore oxide getting appropriate dicyclopentadienyl nickel and Ce modification is placed in the two ends of quartz ampoule, and the load capacity of nickel is 8wt% ~ 12wt%.Vacuumize, under vacuum condition, heating rate is 1 ~ 2 DEG C/min, and 110 ~ 120 DEG C of calcining 20 ~ 24h, are cooled to room temperature, are dissolved in by gained sample in ethanol and stir 4 ~ 5h, with ethanol centrifuge washing 3 ~ 4 times, dry.Under air atmosphere, heating rate is 1 ~ 2 DEG C/min, 500 ~ 600 DEG C of calcining 4 ~ 6h.And then it is reduced, utilize H
2-TPR(hydrogen temperature programmed reduction), first logical N
2pretreatment 30min at 300 DEG C, is cooled to after room temperature with 10%(percent by volume) H
2/ N
2the 1h that reduces at gaseous mixture (30mL/min) 750 DEG C ~ 800 DEG C obtains the dry reforming catalyst of methane of the mesoporous confinement of anti-carbon.
The precursor salt of described cerium is the one in cerous nitrate, cerium chloride, cerous acetate.The modification of different cerium salt pair carriers is different, utilizes the cerium salt mentioned in the present invention to modify mesopore oxide, can make that nano nickel particles is better must be dispersed on mesopore oxide carrier.The size of described nickel metallic particles is at 3-4nm.
Described mesopore oxide carrier is mesoporous silicon sphere, SBA-15, γ-Al
2o
3, the one in KIT-6, MCM-41, these carrier heat-resisting quantities are strong, and in course of reaction, structure is not easily caved in.The mesopore orbit that they have is all relatively more orderly and cell walls is thicker, can nickel particle better must be made to be fixed therein, thus improves anti-sintering property.
In the present invention, the load capacity of cerium is that 3wt% ~ 5wt%, Ce content does not have good modification to carrier very little, and nickel particle can not must be dispersed in mesopore oxide very well, and affects to some extent the anti-carbon performance of catalyst.Ce content is too high, can reduce the interaction force between nickel and carrier, thus nickel particle is easily reunited, and affects catalytic performance.
The calcination process of the nickel-loaded related in the present invention needs to carry out under vacuum.Heating rate is 1 ~ 2 DEG C/min, and calcining heat is 110 ~ 120 DEG C, and calcination time is 20 ~ 24h.Dicyclopentadienyl nickel can distil under vacuum as dicyclopentadienyl nickel steam enters in the duct of mesopore oxide carrier.Programming rate is understood shadow too soon and is played catalyst structure and collapse, and the too low dicyclopentadienyl nickel of calcining heat cannot distil, and the too high meso-hole structure that will cause of temperature is irregular, calcination time too short may dicyclopentadienyl nickel distillation not exclusively, and overlong time can make nickel agglomerate grain.
Compared with prior art, the catalyst tool that prepared by the present invention has the following advantages:
(1) preparation process of the present invention is simple, is easy to operation, and require low to experimental facilities, cost is low, also can not cause secondary pollution to environment.
(2) the inventive method break through traditional aqueous solution wet impregnation method by Ni on carrier, utilize the characteristic of dicyclopentadienyl nickel vacuum sublimation, dicyclopentadienyl nickel steam is made to enter in the duct of mesopore oxide carrier, adding of Ce serves modification to carrier duct inwall, can make that nickel species are better must be dispersed in carrier hole road, thus improve the anti-carbon anti-sintering property of catalyst.
(3) the nanocrystalline size of nickel of catalyst that obtains of the present invention is at about 3nm, and add the confinement effect of carrier mesopore orbit, well can suppress the reunion of the whole middle nickel particle of methane dry weight, reduce the formation of carbon distribution, Ce adds the elimination also contributing to carbon distribution.
Accompanying drawing explanation
Fig. 1 is the whole catalyst n iCe/mSiO of the embodiment of the present invention 1 gained methane dry weight
2transmission electron microscope (TEM) image.
Detailed description of the invention
Specific embodiments of the invention are described in detail below in conjunction with technical scheme and accompanying drawing.
embodiment 1
Take 0.066g cerous nitrate and 0.5g mesoporous silicon sphere is dissolved in deionized water, the load capacity of cerium is 5wt%, mix and blend 8h, dries to obtain the mesoporous silicon sphere modified of Ce.The mesoporous silicon sphere getting 1g dicyclopentadienyl nickel and 0.5g Ce modification is placed in the two ends of quartz ampoule, and the load capacity of nickel is about 10wt%.Vacuumize, under vacuum condition, heating rate is 1 DEG C/min, and 110 DEG C of calcining 24h, are cooled to room temperature, are dissolved in ethanol by gained sample and stir 5h, with ethanol centrifuge washing 3 times, dry.Under air atmosphere, heating rate is 1 DEG C/min, 500 DEG C of calcining 4h.And then it is reduced, utilize H
2-TPR(hydrogen temperature programmed reduction), first logical N
2pretreatment 30min at 300 DEG C, is cooled to after room temperature with 10%(percent by volume) H
2/ N
2the 1h that reduces at gaseous mixture (30mL/min) 800 DEG C obtains NiCe/mSiO
2catalyst.
Test the catalytic activity of above-mentioned catalyst: take 0.15g(40-60 order) catalyst for preparing puts into fixed bed quartz tube reactor and carries out catalyst performance test, CH
4and CO
2sample size is that 1:1(flow is 15mL/min), active testing is from 450 DEG C to 800 DEG C, and at 450 DEG C, catalyst just has certain activity, and at 800 DEG C, activity is the highest, CH
4and CO
2conversion ratio reduciblely respectively reach 94% and 100%.Catalyst stability test is carried out at 750 DEG C, CH after the reaction of 20h
4and CO
2conversion ratio remains on 93% and about 98% respectively, and catalyst still keeps good activity, and the phenomenon of inactivation does not occur.
embodiment 2
Take 0.04g cerium chloride and 0.5g SBA-15 is dissolved in deionized water, the load capacity of cerium is 5wt%, mix and blend 8h, dries to obtain the SBA-15 that modifies of Ce.The SBA-15 getting 1g dicyclopentadienyl nickel and 0.5g Ce modification is placed in the two ends of quartz ampoule, and the load capacity of nickel is about 10wt%.Vacuumize, under vacuum condition, heating rate is 1 DEG C/min, and 120 DEG C of calcining 24h, are cooled to room temperature, are dissolved in ethanol by gained sample and stir 4h, with ethanol centrifuge washing 3 times, dry.Under air atmosphere, heating rate is 1 DEG C/min, 550 DEG C of calcining 4h.And then it is reduced, utilize H
2-TPR, first logical N
2pretreatment 30min at 300 DEG C, is cooled to after room temperature with 10%(percent by volume) H
2/ N
2the 1h that reduces at gaseous mixture (30mL/min) 800 DEG C obtains NiCe/SBA-15 catalyst.
Test the catalytic activity of above-mentioned catalyst: take 0.15g(40-60 order) catalyst for preparing puts into fixed bed quartz tube reactor and carries out catalyst performance test, CH
4and CO
2sample size is that 1:1(flow is 15mL/min), active testing is from 450 DEG C to 800 DEG C, and at 450 DEG C, catalyst just has certain activity, and at 800 DEG C, activity is the highest, CH
4and CO
2conversion ratio reduciblely respectively reach 91% and 98%.Catalyst stability test is carried out at 750 DEG C, CH after the reaction of 20h
4and CO
2conversion ratio remains on 88% and about 94% respectively, and catalyst still keeps good activity, and the phenomenon of inactivation does not occur.
embodiment 3
Take 0.04g cerous nitrate and 0.5g KIT-6 is dissolved in deionized water, the load capacity of cerium is 4wt%, mix and blend 8h, dries to obtain the KIT-6 that modifies of Ce.The KIT-6 getting 1g dicyclopentadienyl nickel and 0.5g Ce modification is placed in the two ends of quartz ampoule, and the load capacity of nickel is about 10wt%.Vacuumize, under vacuum condition, heating rate is 1 DEG C/min, and 110 DEG C of calcining 24h, are cooled to room temperature, are dissolved in ethanol by gained sample and stir 5h, with ethanol centrifuge washing 3 times, dry.Under air atmosphere, heating rate is 1 DEG C/min, 600 DEG C of calcining 4h.And then it is reduced, utilize H
2-TPR, first logical N
2pretreatment 30min at 300 DEG C, is cooled to after room temperature with 10%(percent by volume) H
2/ N
2the 1h that reduces at gaseous mixture (30mL/min) 800 DEG C obtains NiCe/ KIT-6 catalyst.
Test the catalytic activity of above-mentioned catalyst: take 0.15g(40-60 order) catalyst for preparing puts into fixed bed quartz tube reactor and carries out catalyst performance test, CH
4and CO
2sample size is that 1:1(flow is 15mL/min), active testing is from 450 DEG C to 800 DEG C, and at 450 DEG C, catalyst just has certain activity, and at 800 DEG C, activity is the highest, CH
4and CO
2conversion ratio reduciblely respectively reach 93% and 99%.Catalyst stability test is carried out at 750 DEG C, CH after the reaction of 20h
4and CO
2conversion ratio remains on 91% and about 97% respectively, and catalyst still keeps good activity, and the phenomenon of inactivation does not occur.
Claims (4)
1. a preparation method for the dry reforming catalyst of methane of the mesoporous confinement of anti-carbon, is characterized in that having following processing step:
A. the preparation of catalyst: take appropriate cerium precursor salt and mesopore oxide is dissolved in deionized water, the load capacity of cerium is 3wt% ~ 5wt%, mix and blend 7 ~ 8h, dries to obtain the mesopore oxide carrier modified of Ce; The mesopore oxide getting appropriate dicyclopentadienyl nickel and Ce modification is placed in the two ends of quartz ampoule, and the load capacity of nickel is 8wt% ~ 12wt%; Vacuumize, under vacuum condition, heating rate is 1 ~ 2 DEG C/min, and 110 ~ 120 DEG C of calcining 20 ~ 24h, are cooled to room temperature, are dissolved in by gained sample in ethanol and stir 4 ~ 5h, with ethanol centrifuge washing 3 ~ 4 times, dry; Under air atmosphere, heating rate is 1 ~ 2 DEG C/min, 500 ~ 600 DEG C of calcining 4 ~ 6h;
B. the reduction of catalyst: utilize H
2-TPR, first logical N
2pretreatment 30min at 300 DEG C, is cooled to after room temperature with H
2/ N
2percent by volume is the gaseous mixture of 10%, and flow velocity is 30mL/min, and the 1h that reduces at 750 DEG C ~ 800 DEG C obtains the dry reforming catalyst of methane of the mesoporous confinement of anti-carbon.
2., according to the preparation method of the dry reforming catalyst of methane of the mesoporous confinement of anti-carbon described in claims 1, it is characterized in that described cerium precursor salt is the one in cerous nitrate, cerium chloride, cerous acetate.
3., according to the preparation method of the dry reforming catalyst of methane of the mesoporous confinement of anti-carbon described in claims 1, it is characterized in that described mesoporous material is mesoporous silicon sphere, SBA-15, γ-Al
2o
3, the one in KIT-6, MCM-41.
4. according to the preparation method of the dry reforming catalyst of methane of the mesoporous confinement of anti-carbon described in claims 1, it is characterized in that the size of described nickel metallic particles is at 3-4nm, utilize dicyclopentadienyl nickel vacuum sublimation to be that nickel steam enters in carrier mesopore orbit.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105944730A (en) * | 2016-05-13 | 2016-09-21 | 南昌大学 | Preparation method of mesopore confined nickel-based methane reforming catalyst |
| CN105964259A (en) * | 2016-05-13 | 2016-09-28 | 南昌大学 | {0><}0{>Preparation method of polynuclear core-shell structure nickel-based catalyst |
| CN110292927A (en) * | 2019-04-30 | 2019-10-01 | 北京氦舶科技有限责任公司 | Monoatomic metal catalyst and its preparation and the application in degradation air pollutants |
| CN112403466A (en) * | 2020-11-06 | 2021-02-26 | 上海簇睿低碳能源技术有限公司 | Preparation method of core-shell catalyst for dry reforming of methane and carbon dioxide |
| CN113000059A (en) * | 2021-02-04 | 2021-06-22 | 上海大学 | Nickel-based catalyst for dry reforming of methane and carbon dioxide and preparation method and application thereof |
| CN115282970A (en) * | 2022-08-03 | 2022-11-04 | 高潞空气化工产品(上海)能源科技有限公司 | Nickel-based catalyst for oxide film limited low-carbon alkane dry reforming and preparation method and application thereof |
| CN115518652A (en) * | 2022-06-13 | 2022-12-27 | 安徽理工大学 | Silicon-cerium composite microporous material packaged metal catalyst and preparation method and application thereof |
| CN116371451A (en) * | 2023-04-14 | 2023-07-04 | 西安交通大学 | Cerium doped nickel-based catalyst suitable for methane dry reforming and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105944730A (en) * | 2016-05-13 | 2016-09-21 | 南昌大学 | Preparation method of mesopore confined nickel-based methane reforming catalyst |
| CN105964259A (en) * | 2016-05-13 | 2016-09-28 | 南昌大学 | {0><}0{>Preparation method of polynuclear core-shell structure nickel-based catalyst |
| CN110292927A (en) * | 2019-04-30 | 2019-10-01 | 北京氦舶科技有限责任公司 | Monoatomic metal catalyst and its preparation and the application in degradation air pollutants |
| CN112403466A (en) * | 2020-11-06 | 2021-02-26 | 上海簇睿低碳能源技术有限公司 | Preparation method of core-shell catalyst for dry reforming of methane and carbon dioxide |
| CN112403466B (en) * | 2020-11-06 | 2023-01-03 | 上海簇睿低碳能源技术有限公司 | Preparation method of core-shell catalyst for dry reforming of methane and carbon dioxide |
| CN113000059A (en) * | 2021-02-04 | 2021-06-22 | 上海大学 | Nickel-based catalyst for dry reforming of methane and carbon dioxide and preparation method and application thereof |
| CN115518652A (en) * | 2022-06-13 | 2022-12-27 | 安徽理工大学 | Silicon-cerium composite microporous material packaged metal catalyst and preparation method and application thereof |
| CN115282970A (en) * | 2022-08-03 | 2022-11-04 | 高潞空气化工产品(上海)能源科技有限公司 | Nickel-based catalyst for oxide film limited low-carbon alkane dry reforming and preparation method and application thereof |
| CN115282970B (en) * | 2022-08-03 | 2023-12-08 | 高潞空气化工产品(上海)能源科技有限公司 | Nickel-based catalyst for oxide film limited-area low-carbon alkane dry reforming and preparation method and application thereof |
| CN116371451A (en) * | 2023-04-14 | 2023-07-04 | 西安交通大学 | Cerium doped nickel-based catalyst suitable for methane dry reforming and preparation method thereof |
| CN116371451B (en) * | 2023-04-14 | 2024-05-17 | 西安交通大学 | Cerium doped nickel-based catalyst suitable for methane dry reforming and preparation method thereof |
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Application publication date: 20150819 |