CN108273508A - A kind of preparation method of high-performance reforming of methane on Ni-Ce nickel-base catalyst - Google Patents
A kind of preparation method of high-performance reforming of methane on Ni-Ce nickel-base catalyst Download PDFInfo
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- CN108273508A CN108273508A CN201810166111.8A CN201810166111A CN108273508A CN 108273508 A CN108273508 A CN 108273508A CN 201810166111 A CN201810166111 A CN 201810166111A CN 108273508 A CN108273508 A CN 108273508A
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- 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
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- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
- C01B3/40—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts characterised by the catalyst
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Abstract
Nickel nitrate is first reacted synthesis nickel hydroxide powder, then complex prepared by nickel hydroxide and glycine as presoma, with SiO by a kind of preparation method of high-performance reforming of methane on Ni-Ce nickel-base catalyst, this method with NaOH2Or Al2O3As carrier, the methane reforming nickel-base catalyst of high activity and high stability is prepared for using excessive infusion process（Ni/SiO2Or Ni/Al2O3）.The present invention has raw material nickel nitrate, NaOH, glycine and the carrier prepared used in catalyst（SiO2Or Al2O3）It is cheap and easy to get, the advantages that preparation process condition is simple, is easily industrialized, and repeatability is good.Compared with traditional dipping technique, catalyst prepared by the method for the present invention not only shows higher CH4Conversion ratio, and there is very high stability, significantly improve the activity and stability of methane reforming reaction.
Description
Technical field
The invention belongs to catalyst technical fields, and in particular to a kind of high-performance reforming of methane on Ni-Ce nickel-base catalyst
Preparation method.
Background technology
As people go deep into greenhouse effects understanding, the CO as most one of strong greenhouse gas2Capture and its effectively
Using causing increasingly extensive attention.Wherein, with natural gas or coal bed gas（Main component is methane）Clean utilization mutually tie
The CO of conjunction2With CH4It reforms（CDR）Preparing synthetic gas or hydrogen technology have been a great concern, and conduct extensive research report.
CDR processes utilize CO simultaneously2And CH4Two big greenhouse gases, are of great significance to reduction of greenhouse gas discharge, and the H of synthesis gas2/CO
≤ 1, it can be used as carbonyl and organic oxygen-containing compound synthesis and through Fischer-Tropsch（FT）Synthetic reaction synthesizes the raw material of long-chain hydro carbons
Gas.Importantly, with other CO2Trans-utilization technology is compared, and CDR is expected to directly apply to CH4With CO in flue gas2Weight
Whole reaction, without to CO in flue gas2Carry out pre-separation.Therefore, the process of industrialization of CDR reactions is for solving energy problem
And realize CO2Emission reduction and efficient utilize all have significance.Studies have shown that catalyst inactivation caused by carbon deposit and sintering is
The bottleneck of CDR industrial applications.Therefore, numerous studies have been carried out around the stability of catalyst.
The study found that in addition to Os, VIII group 4 transition metal all has catalytic activity, wherein noble metal to methane reforming reaction
（Such as Pt, Pd, Rh, Ir）Catalytic activity it is higher, anti-carbon deposition ability is stronger, and stability is preferable.But consider catalytic performance
And economy, Ni base catalyst are optimal.Therefore, how to improve the performance of Ni base catalyst, especially stability becomes currently
One of research hotspot.
Comprehensive analysis pertinent literature is reported it can be found that influencing the key factor master of Ni base catalyst carbon depositions in CDR reactions
That is, it the particle size of Ni and its to interact with carrier there are two aspect.Studies have shown that short grained Ni can effectively inhibit
The generation of carbon distribution, but after Ni particle sizes increase to 9 nm or more, the carbon deposition rate of catalyst surface can be accelerated rapidly, to
Lead to catalyst inactivation.Therefore, it obtains the Ni base catalyst of high dispersive, and is interacted to inhibit by increasing it between carrier
Its sintering of Ni under high temperature reduction and reaction condition can effectively control the generation of carbon distribution.For above-mentioned influence Ni base catalyst
The key factor of performance, domestic and international scientific research personnel take a variety of new strategies to improve the anti-sintering of Ni base catalyst and anti-carbon
Can, for example, synthesis core shell structure catalyst or nanometer confinement type catalyst, pass through modulation Ni particle sizes and its phase between carrier
A large amount of innovative researches have been carried out in terms of interaction, and have achieved certain effect.
Invention content
For overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of high-performance reforming of methane on Ni-Ce nickel
The preparation method of base catalyst, using the stable complex of nickel hydroxide and Formation of glycine as presoma, SiO2Or Al2O3To carry
Body is prepared for the methane reforming nickel-base catalyst of high activity and high stability by excessive infusion process.Compared with traditional infusion process,
The catalyst prepared using the present invention can significantly improve the activity of methane reforming reaction, especially stability.
To achieve the goals above, the technical solution adopted by the present invention is：
A kind of preparation method of high-performance reforming of methane on Ni-Ce nickel-base catalyst, includes the following steps：
1）Under the conditions of being stirred at room temperature, 0.2 mol/L NaOH aqueous solutions are added drop-wise in 0.1 mol/L nickel nitrate aqueous solutions, are dripped
It stirs 30~60 minutes, centrifuges after adding, deionized water is washed till neutrality, and 80~120 DEG C of dryings 10~12 hours are ground
To nickel hydroxide powder；
2）Under 50~80 DEG C of stirring conditions, nickel hydroxide powder is added to the glycine solution of 0.01~0.1 g/mL
In, continue stirring 1~4 hour, obtains nickel glycinate complex solution；
3）According to Ni load capacity 5%~20%, by SiO2Or Al2O3It is added in nickel glycinate complex solution, in 50~80 DEG C of items
It is stirred under part 0.5~1.5 hour, then removes water at 50~80 DEG C with Rotary Evaporators, 80~120 DEG C of dryings 10~12 are small
When, 500 DEG C roast 4 hours, and tabletting, granulation, the particle for screening 40~60 mesh, obtain nickel-base catalyst after roasting.
The step 1）The molar ratio of middle nickel nitrate and NaOH are 1:2~2.5.
The step 2）The molar ratio of middle nickel hydroxide and glycine is 1:2~3.
The step 3）Middle whipping temp is to stir 1-1.5 hours under the conditions of 80 DEG C.
The step 3）Middle roasting rises to 500 DEG C with 5 DEG C/min of heating rate and roasts 4 hours.
The beneficial effects of the invention are as follows：
The present invention is using the stable complex of nickel hydroxide and Formation of glycine as presoma, SiO2Or Al2O3For carrier, passed through
Amount infusion process is prepared for the methane reforming nickel-base catalyst of high activity and high stability.Compared with traditional infusion process, this hair is used
The catalyst of bright preparation can significantly improve the activity of methane reforming reaction, especially stability.
It is cheap and easy to get that the present invention prepares the raw material used in catalyst, and preparation process is simple, is easily industrialized, and has
Good repeatability.
Specific implementation mode
With reference to embodiment, the present invention is described in more detail, but protection scope of the present invention is not limited only to these realities
Apply example.
Embodiment 1
Under the conditions of being stirred at room temperature, 25 mL, 0.2 mol/L NaOH aqueous solutions are added drop-wise to 25 mL, 0.1 mol/L nickel nitrates
In aqueous solution, continue stirring 60 minutes after dripping, centrifuge, deionized water is washed till neutrality, and 100 DEG C of dryings 12 hours obtain
To nickel hydroxide powder.According to Ni load capacity 10%, under 80 DEG C of stirring conditions, 0.1755 g nickel hydroxide powders are added to
In the glycine solution of 8.6 mL, 0.05 g/mL（The molar ratio of glycine and nickel hydroxide is 3）, continue stirring 2 hours,
Obtain nickel glycinate complex dipping solution.1.00 g SiO are added in nickel glycinate complex dipping solution again2, in 80 DEG C of items
It stirs 1 hour under part, then removes water at 50 DEG C with Rotary Evaporators, 80 DEG C of dryings 12 hours, with 5 DEG C/min of heating speed
Rate rises to 500 DEG C and roasts 4 hours, and tabletting, granulation, the particle for screening 40~60 mesh obtain nickel-base catalyst.
Embodiment 2
Under the conditions of being stirred at room temperature, 30 mL, 0.2 mol/L NaOH aqueous solutions are added drop-wise to 20 mL, 0.1 mol/L nickel nitrates
In aqueous solution, continue stirring 30 minutes after dripping, centrifuge, deionized water is washed till neutrality, and 120 DEG C of dryings 10 hours obtain
To nickel hydroxide powder.According to Ni load capacity 5%, under 80 DEG C of stirring conditions, 0.0831 g nickel hydroxide powders are added to 13
In the glycine solution of 0.01 g/mL of mL（The molar ratio of glycine and nickel hydroxide is 2）, continue stirring 2 hours, obtain
Nickel glycinate complex dipping solution.1.00 g SiO are added in nickel glycinate complex dipping solution again2, under the conditions of 80 DEG C
Then stirring 1 hour removes water at 60 DEG C with Rotary Evaporators, 100 DEG C of dryings 12 hours, with 5 DEG C/min of heating rate
It rises to 500 DEG C to roast 4 hours, tabletting, granulation, the particle for screening 40~60 mesh obtain nickel-base catalyst.
Embodiment 3
Under the conditions of being stirred at room temperature, 25 mL, 0.2 mol/L NaOH aqueous solutions are added drop-wise to 25 mL, 0.1 mol/L nickel nitrates
In aqueous solution, continue stirring 30 minutes after dripping, centrifuge, deionized water is washed till neutrality, and 100 DEG C of dryings 12 hours obtain
To nickel hydroxide powder.According to Ni load capacity 10%, under 80 DEG C of stirring conditions, 0.1755 g nickel hydroxide powders are added to
In the glycine solution of 5.7 mL, 0.10 g/mL（The molar ratio of glycine and nickel hydroxide is 4）, continue stirring 1 hour,
Obtain nickel glycinate complex dipping solution.1.00 g SiO are added in nickel glycinate complex dipping solution again2, at 100 DEG C
Under the conditions of stir 1 hour, then remove water at 70 DEG C with Rotary Evaporators, 120 DEG C of dryings 10 hours, with 5 DEG C/min of liter
Warm rate rises to 500 DEG C and roasts 4 hours, and tabletting, granulation, the particle for screening 40~60 mesh obtain nickel-base catalyst.
Embodiment 4
Under the conditions of being stirred at room temperature, 50 mL, 0.2 mol/L NaOH aqueous solutions are added drop-wise to 50 mL, 0.1 mol/L nickel nitrates
In aqueous solution, continue stirring 60 minutes after dripping, centrifuge, deionized water is washed till neutrality, and 80 DEG C of dryings 12 hours obtain
Nickel hydroxide powder.According to Ni load capacity 20%, under 80 DEG C of stirring conditions, 0.3949 g nickel hydroxide powders are added to 4.0
In the glycine solution of 0.08 g/mL of mL（The molar ratio of glycine and nickel hydroxide is 1）, continue stirring 0.5 hour, obtain
To nickel glycinate complex dipping solution.1.00 g SiO are added in nickel glycinate complex dipping solution again2, in 100 DEG C of items
It stirs 1 hour under part, then removes water at 80 DEG C with Rotary Evaporators, 100 DEG C of dryings 12 hours, with 5 DEG C/min of heating
Rate rises to 500 DEG C and roasts 4 hours, and tabletting, granulation, the particle for screening 40~60 mesh obtain nickel-base catalyst.
Embodiment 5
Under the conditions of being stirred at room temperature, 50 mL, 0.2 mol/L NaOH aqueous solutions are added drop-wise to 50 mL, 0.1 mol/L nickel nitrates
In aqueous solution, continue stirring 60 minutes after dripping, centrifuge, deionized water is washed till neutrality, and 120 DEG C of dryings 10 hours obtain
To nickel hydroxide powder.According to Ni load capacity 15%, under 80 DEG C of stirring conditions, 0.2787 g nickel hydroxide powders are added to
In the glycine solution of 9.0 mL, 0.05 g/mL（The molar ratio of glycine and nickel hydroxide is 2）, continue stirring 1 hour,
Obtain nickel glycinate complex dipping solution.1.00 g Al are added in nickel glycinate complex dipping solution again2O3, at 100 DEG C
Under the conditions of stir 1 hour, then remove water at 60 DEG C with Rotary Evaporators, 80 DEG C of dryings 12 hours, with 5 DEG C/min of liter
Warm rate rises to 500 DEG C and roasts 4 hours, and tabletting, granulation, the particle for screening 40~60 mesh obtain nickel-base catalyst.
Embodiment 6
Under the conditions of being stirred at room temperature, 25 mL, 0.2 mol/L NaOH aqueous solutions are added drop-wise to 25 mL, 0.1 mol/L nickel nitrates
In aqueous solution, continue stirring 60 minutes after dripping, centrifuge, deionized water is washed till neutrality, and 100 DEG C of dryings 12 hours obtain
To nickel hydroxide powder.According to Ni load capacity 10%, under 80 DEG C of stirring conditions, 0.1755 g nickel hydroxide powders are added to
In the glycine solution of 5.4 mL, 0.08 g/mL（The molar ratio of glycine and nickel hydroxide is 3）, it is small to continue stirring 0.5
When, obtain nickel glycinate complex dipping solution.1.00 g Al are added in nickel glycinate complex dipping solution again2O3, 100
It stirs 2 hours under the conditions of DEG C, then removes water at 60 DEG C with Rotary Evaporators, 100 DEG C of dryings 12 hours, with 5 DEG C/min
Heating rate rises to 500 DEG C and roasts 4 hours, and tabletting, granulation, the particle for screening 40~60 mesh obtain nickel-base catalyst.
In order to verify beneficial effects of the present invention, inventor has carried out performance to nickel-base catalyst prepared by Examples 1 to 6
Evaluation, specific experiment situation are as follows：
0.10 g catalyst is placed in fixed bed reactors, is passed through the H that volume ratio is 20% in atmospheric conditions2/N2, flow
For 50 mLmin-1, with 4 DEG C of min-1Heating rate rise to 700 DEG C from room temperature, reductase 12 .5 hours.Then, it closes
H2, continue to be passed through N2, with 2 DEG C of min-1Heating rate be warming up to 750 DEG C, after temperature stabilization after, be switched to reaction gas（CO2
With CH4Volume ratio be 1: 1 gaseous mixture）, the total amount of reaction gas is 100 mLmin-1, P=1.0 atm, T=
750 DEG C, CO2/CH4=1.0, the mLg of air speed=60000-1·h-1Under the conditions of react, the gas after reaction is stood by Zhejiang good fortune
The chromatograph of II type thermal conductivity cell detectors of GC9720（Chromatographic column is 5A and PQ columns）Detection and analysis.Experimental result is shown in Table 1.
The CH4 production performance of 1 different catalysts of table
| Catalyst | Methane initial conversion（%） | Carbon dioxide initial conversion（%） | Methane conversion after 20 hours（%） | Carbon dioxide conversion after 20 hours（%） |
| Embodiment 1 | 84.7 | 93.8 | 83.2 | 93.1 |
| Embodiment 2 | 80.6 | 90.1 | 78.5 | 88.3 |
| Embodiment 3 | 80.5 | 91.7 | 77.6 | 89.5 |
| Embodiment 4 | 85.1 | 94.5 | 70.6 | 79.7 |
| Embodiment 5 | 82.6 | 93.1 | 82.0 | 90.9 |
| Embodiment 6 | 83.0 | 92.1 | 82.1 | 90.2 |
As shown in Table 1, the Ni/SiO that prepared by the method for the present invention2And Ni/Al2O3Catalyst all has methane reforming reaction higher
Reactivity, CH4And CO2Initial conversion is up to 80% and 90% or more respectively.After reaction 20 hours, CH4And CO2Conversion ratio
Remain above 70% and 79%.
Claims (5)
1. a kind of preparation method of high-performance reforming of methane on Ni-Ce nickel-base catalyst, which is characterized in that include the following steps：
1）Under the conditions of being stirred at room temperature, 0.2 isometric mol/L NaOH aqueous solutions are added drop-wise to 0.1 mol/L nickel nitrate water
In solution, continue stirring after being added dropwise to complete 30~60 minutes, centrifuges solid, then be washed with deionized water to neutrality, 80~
It is 10~12 hours dry in 120 DEG C of baking ovens, nickel hydroxide powder is obtained after grinding；
2）Under 50~80 DEG C of stirring conditions, nickel hydroxide powder is added to the glycine solution of 0.01~0.1 g/mL
In, continue stirring 1~4 hour, obtains nickel glycinate complex solution；
3）According to Ni load capacity 5%~20%, by SiO2Or Al2O3It is added in nickel glycinate complex solution, in 50~80 DEG C of items
Continue stirring under part 0.5~1.5 hour, then removes water, 80~120 DEG C of dryings 10~12 at 50~80 DEG C with Rotary Evaporators
Hour, 500 DEG C roast 4 hours, and tabletting, granulation, the particle for screening 40~60 mesh, obtain Ni/SiO after roasting2Or Ni/Al2O3It urges
Agent.
2. a kind of preparation method of high-performance reforming of methane on Ni-Ce nickel-base catalyst according to claim 1, special
Sign is, the step 1）The molar ratio of middle nickel nitrate and NaOH are 1:2~2.5.
3. a kind of preparation method of high-performance reforming of methane on Ni-Ce nickel-base catalyst according to claim 1, special
Sign is, the step 2）The molar ratio of middle nickel hydroxide and glycine is 1:2~3.
4. the preparation method of high-performance methane reforming nickel-base catalyst according to claim 1, which is characterized in that described
Step 3）Middle whipping temp is to stir 1-1.5 hours under the conditions of 80 DEG C.
5. the preparation method of high-performance methane reforming nickel-base catalyst according to claim 1, which is characterized in that described
Step 3）Middle roasting rises to 500 DEG C with 5 DEG C/min of heating rate and roasts 4 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110270377A (en) * | 2019-07-01 | 2019-09-24 | 西京学院 | A kind of methane dry reforming nickel-base catalyst and its preparation method and application |
| CN110813341A (en) * | 2019-11-21 | 2020-02-21 | 浙江科技学院 | Methane dry reforming reaction catalyst and preparation method and application thereof |
| CN111495376A (en) * | 2020-05-13 | 2020-08-07 | 南京大学 | Pod-shaped load type Ni/Al2O3Catalyst, preparation method and application thereof |
| CN113512737A (en) * | 2021-04-01 | 2021-10-19 | 安徽大学 | Nickel hydroxide electrocatalyst, preparation method, electrochemical activation method and application thereof |
| CN116139910A (en) * | 2023-02-15 | 2023-05-23 | 昆明理工大学 | New use of nickel-based re-hydroxylation silicon-based catalyst |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110270377A (en) * | 2019-07-01 | 2019-09-24 | 西京学院 | A kind of methane dry reforming nickel-base catalyst and its preparation method and application |
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| CN110813341B (en) * | 2019-11-21 | 2022-09-09 | 浙江科技学院 | Methane dry reforming reaction catalyst and preparation method and application thereof |
| CN111495376A (en) * | 2020-05-13 | 2020-08-07 | 南京大学 | Pod-shaped load type Ni/Al2O3Catalyst, preparation method and application thereof |
| CN113512737A (en) * | 2021-04-01 | 2021-10-19 | 安徽大学 | Nickel hydroxide electrocatalyst, preparation method, electrochemical activation method and application thereof |
| CN113512737B (en) * | 2021-04-01 | 2022-07-19 | 安徽大学 | Nickel hydroxide electrocatalyst, preparation method, electrochemical activation method and application thereof |
| CN116139910A (en) * | 2023-02-15 | 2023-05-23 | 昆明理工大学 | New use of nickel-based re-hydroxylation silicon-based catalyst |
| CN116139910B (en) * | 2023-02-15 | 2024-03-22 | 昆明理工大学 | New use of nickel-based re-hydroxylation silicon-based catalyst |
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Application publication date: 20180713 |