CN104383924A - Composite nanometer nickel-based catalyst, preparation and application method thereof - Google Patents
Composite nanometer nickel-based catalyst, preparation and application method thereof Download PDFInfo
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- CN104383924A CN104383924A CN201410490319.7A CN201410490319A CN104383924A CN 104383924 A CN104383924 A CN 104383924A CN 201410490319 A CN201410490319 A CN 201410490319A CN 104383924 A CN104383924 A CN 104383924A
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Abstract
The present invention relates to a composite nanometer nickel-based catalyst, preparation and an application method thereof. The composite nanometer nickel-based catalyst comprises dolomite and a nickel-based catalyst, wherein the nickel-based catalyst is a nickel oxide/alumina catalyst. According to the preparation, a coordination uniform precipitation method is adopted, nickel nitrate hexahydrate is adopted as a raw material, ammonia water is adopted as a coordination agent to prepare a nickel oxide precursor, nickel hydroxide precipitation is performed, and then the nickel hydroxide is loaded in the hole substance gamma-Al2O3 so as to obtain the nickel-based catalyst. During the application, dolomite and the nickel-based catalyst are added to garbage, and cracking gasification is performed at a high temperature so as to remove tar produced during the garbage cracking process. With the composite nanometer nickel-based catalyst, the gas yield of the municipal solid waste material and the hydrogen production rate of the produced gas can be significantly improved, and the tar substance can be effectively removed.
Description
Technical field
The present invention relates to a kind of catalyst of efficient pyrolysis gasification, be specifically related to a kind of nickel-base catalyst and preparation and application method thereof.
Background technology
A large amount of uses of fossil energy create severe environmental problem, and health and the existence of the mankind in serious threat.The dual-pressure of energy crisis and environmental pollution forces people to re-recognize to be needed to find regenerative resource, with progressively substitute fossil fuels, alleviates energy shortage and environmental pollution.At present, the quick growth of domestic waste discharge capacity brings new environmental problem.In these domestic waste pyrolysis gasification processing procedures, existence product hydrogen rate is low, gasification efficiency is not high and a large amount of tar produced problem, these tar can cause the corrosion of equipment and the blocking of pipeline in the application process of combustion gas, have a strong impact on the normal operation of biomass gasification system and the utilization of combustion gas.And the removal of tar is the heavy difficulties that the research of current garbage cracking gasification technology will solve.In addition, in current domestic waste pyrolysis gasification processing procedure, also exist and produce the problem that hydrogen rate is low, gasification efficiency is not high, address these problems.
Summary of the invention
The object of this invention is to provide a kind of composite nano nickel-base catalyst and preparation and application method thereof, Coordination homogeneous precipitation method is adopted effectively to prepare nickel-base catalyst, it can significantly improve the gas production of domestic waste material and the product hydrogen rate of aerogenesis, and effectively can remove tar material.
The object of the invention is to be achieved through the following technical solutions:
A kind of composite nano nickel-base catalyst, described composite nano nickel-base catalyst comprises dolomite and nickel-base catalyst, and the mass ratio of the two is: 15 ~ 30: 75 ~ 85; Described nickel-base catalyst is loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst.Al herein
2o
3preferred γ-Al
2o
3.
Further preferably, described dolomite is the dolomite after calcining.
Further preferably, the mass ratio of described dolomite and nickel-base catalyst is: 1: 4.
A preparation method for described composite nano nickel-base catalyst, its preparation method comprises the following steps:
1. dolomite is carried out calcining 8 ~ 30 minutes being not less than at 1000 DEG C, obtain the dolomite after calcining;
2. with Nickelous nitrate hexahydrate [Ni (NO
3)
26H
2o] be raw material, and add complexant, then at 180 ~ 300 DEG C, adopt Coordination homogeneous precipitation legal system for nano NiO presoma; Described Nickelous nitrate hexahydrate [Ni (NO
3)
26H
2o] and the ratio of ammoniacal liquor be 10.17 ~ 17.8g/100mL;
3. γ-Al2O3 carrier, nano NiO presoma and surfactant is added, 1 ~ 1.5h is calcined at 400 ~ 450 DEG C, the nano NiO presoma of load on γ-Al2O3 particle is decomposed into nano-nickel oxide (NiO), and then can obtain loaded nano nickel oxide/alumina (NiO/ γ-Al
2o
3) catalyst;
4. by step 1. in dolomite after calcining and step 3. in the loaded nano nickel oxide/alumina (NiO/ γ-Al of gained
2o
3) catalyst mix obtains described composite nano nickel-base catalyst.
Further preferably, step 2. middle Nickelous nitrate hexahydrate [Ni (NO
3)
26H
2o] and the complexant temperature that is prepared nano NiO presoma be 220 ~ 260 DEG C.
Further preferably, the Nickelous nitrate hexahydrate of 100mL ammoniacal liquor and 15g ~ 16g reacts.
Further preferably, described complexant is ammoniacal liquor.
Further preferably, described ammoniacal liquor is the ammoniacal liquor after the dilution adding 3 times of volume water gagings in ammoniacal liquor.
Further preferably, step 2. described in Nickelous nitrate hexahydrate [Ni (NO
3)
26H
2o] and the ratio of ammoniacal liquor be 15 ~ 16g/100mL.
Further preferably, described NiO presoma is nickel hydroxide.
Further preferably, step 3. in add surfactant.
Further preferably, step 3. in uniform load nano-nickel oxide (NiO) on alumina support, the thickness of this nano-nickel oxide (NiO) layer is 8 ~ 500 μm.
Further preferably, the nano-nickel oxide of load on described alumina support is be made up of some nickel oxide (NiO) nanometer sheet, this nickel oxide (NiO) nanometer sheet is upright interlaced growth on the alumina support, and the thickness of this nickel oxide (NiO) nanometer sheet is 40nm-3 μm.
An application process for described composite nano nickel-base catalyst, is characterized in that: described application process comprises the following steps: S1: house refuse be added in pyrolysis gasification reactor; S2: by the dolomite after calcining and loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst is added in mass ratio in house refuse and carries out pyrolysis gasification at 600 DEG C ~ 900 DEG C, can remove the tar produced in garbage cracking process.
Further preferably, in step S2, the temperature of house refuse pyrolysis gasification is preferably 800 DEG C.
The invention provides a kind of composite nano nickel-base catalyst and preparation and application method thereof, its beneficial effect mainly had is: the application adopts Coordination homogeneous precipitation method effectively to prepare nickel-base catalyst, this composite nano nickel-base catalyst can significantly improve the gas production of domestic waste material and the product hydrogen rate of aerogenesis, and effectively can remove tar material.
Accompanying drawing explanation
With reference to the accompanying drawings the present invention is described in further detail below.
Fig. 1 is the preparation flow figure of the composite nano nickel-base catalyst described in the embodiment of the present invention;
Fig. 2 is the reaction principle figure of the Coordination homogeneous precipitation method described in the embodiment of the present invention;
Fig. 3 is the Ni (OH) described in the embodiment of the present invention
2the XRD figure of precipitation;
Fig. 4 is the XRD figure of the nickel oxide particle described in the embodiment of the present invention;
Fig. 5 is the XRD figure of the nano-nickel oxide/aluminium oxide catalyst described in the embodiment of the present invention.
Detailed description of the invention
For specific experiment case, detailed description of the invention is described below, should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention, Fig. 1 is the preparation flow of the nickel-base catalyst of this experiment.
Embodiment 1: the preparation principle of nickel-base catalyst
The method that this experiment adopts is Coordination homogeneous precipitation method, the general principle of Coordination homogeneous precipitation method first metal ion and corresponding complexant is reacted, generate corresponding complex solution, by changing the condition of reaction system, complex being balanced and moves to direction of dissociating.After metal ion in solution is accumulated to finite concentration, just can reacts to generate with the precipitating reagent in solution system and precipitate.The method of the ultra-fine uniformed powder of this preparation needs special setting uniform stirring system, thus ensure that metal ion and precipitating reagent can distribute equably in whole system, only in this way the whole system of guarantee can generate equably and separate out precipitation, so just can effectively avoid ion distribution uneven, if local over-concentration, easily produce the phenomenon of particle agglomeration, uniform stirring system also can be good at the grain diameter controlling precipitated product simultaneously.
The ammoniacal liquor that the present invention selects market at prices cheap is as complexant, Nickelous nitrate hexahydrate is experimental raw, after both react generating nickel amine complex solution, by being diluted with water solution concentration, and the method for ammonia is driven away in heating, the complex balance of the nickel ammonia solution that reaction is generated moves to dissociation direction.In whole solution system, dissociation nickel ion out and precipitating reagent OH-rely on the existence of this stirring system and are uniformly distributed, and therefore hydroxide ion can reach more sufficient hybrid reaction with nickel ion.The key reaction process of whole reaction as shown in Figure 2.
Embodiment 2:Ni (OH)
2preparation process
In the application, first the preparation of nickel-base catalyst chooses Nickelous nitrate hexahydrate [Ni (NO
3)
26H
2o] as raw material, ammoniacal liquor, as complexant, takes the Nickelous nitrate hexahydrate particle of 10.17g, then the distilled water of 50mL is added, utilize agitator to stir uniformly, continue 5min, when nickel nitrate solution mixes, just bright-coloured bottle green is presented, now measure the ammoniacal liquor of 100mL, join nickel nitrate solution, solution reacts at once becomes navy blue nickel amine complex solution, add 100mL distilled water again, continue to stir 5min.The nickel amine complex solution stirred is transferred in the three-neck flask of 1000mL.Before experiment starts, need to have debugged the temperature shelves of electric food warmer and the mixing speed of agitator, then the three-neck flask having contained solution is put into electric food warmer, fix three necks.Middle flask bottleneck is fixing with agitator, and the bottleneck of side is fixing with snakelike return duct, and opposite side is closed, thus prevents ammoniacal liquor from high temperature excessively volatilizing.Open electric mixer, make agitator uniform stirring in the solution of three-neck flask, then open electric food warmer, heat, continue 1.5h.This tests the Ni (OH) under all preparation conditions
2all tested by laser particle size analysis, determine its particle diameter such as particle diameter and specific area situation.This experiment adopts suction filtration machine to be separated in three-neck flask the precipitation of reacting precipitation, by the solution that is obtained by reacting by qualitative filter paper (middling speed) suction filtration, obtains a large amount of Ni (OH)
2powder, the precipitation obtained by suction filtration puts into the dry 8h of drying box, takes out dried powder, weighs.
1,15.26g Nickelous nitrate hexahydrate [Ni (NO is taken
3)
26H
2o], add 100mL ammoniacal liquor, and add the distilled water of 300mL, then prepare nano NiO presoma at 220 DEG C, dry, weigh, obtain nano NiO presoma [i.e. Ni (OH)
2] 4.2218g;
2,10.17g Nickelous nitrate hexahydrate [Ni (NO is taken
3)
26H
2o], add 100mL ammoniacal liquor, and add the distilled water of 300mL, then prepare nano NiO presoma at 300 DEG C, dry, weigh, obtain nano NiO presoma [i.e. Ni (OH)
2] 3.8718g;
3,17.8g Nickelous nitrate hexahydrate [Ni (NO is taken
3)
26H
2o], add 100mL ammoniacal liquor, and add the distilled water of 300mL, then prepare nano NiO presoma at 260 DEG C, dry, weigh, obtain nano NiO presoma [i.e. Ni (OH)
2] 4.2708g;
4,14.26g Nickelous nitrate hexahydrate [Ni (NO is taken
3)
26H
2o], add 80mL ammoniacal liquor, and add the distilled water of 240mL, then prepare nano NiO presoma at 240 DEG C, dry, weigh, obtain nano NiO presoma [i.e. Ni (OH)
2] 3.9612g.
By the NiO precursor prepared, i.e. Ni (OH)
2precipitation does deep XRD and scanning electron microscope analysis respectively.And the analysis result obtained is carried out corresponding Analysis on Mechanism.Ni (OH)
2the XRD test result figure of precipitation as shown in Figure 3; Analysis report according to above XRD shows, and all elements of material contains H, O and Ni, can be seen by collection of illustrative plates, the XRD collection of illustrative plates of material and Ni (OH)
2reference material one_to_one corresponding, and there is no the appearance of assorted peak, prove that this material prepared is exactly the Ni (OH) that will obtain
2particle.
Embodiment 3: the preparation of nickel oxide NiO
1. react the dry Ni (OH) 2 prepared, just the presoma of nickel-base catalyst, obtain nickel oxide particle, first can put into Muffle furnace, 400 DEG C or temperature lower calcination 2h, such Ni (OH) 2 pyrolytic, thus obtain the nickel oxide NiO of black.
2. Ni (OH) 2 powder reacting the drying prepared is put into crucible, send into Muffle furnace, at the temperature lower calcination 1h of 430 DEG C, then the powder obtained is nickel oxide to be prepared.
Nickel oxide NiO obtained above is done deep XRD and scanning electron microscope analysis, and Fig. 4 is the XRD test result of nickel oxide particle.The mean grain size that can obtain nickel oxide particle corresponding to upper figure according to Scherrer formula is: 51.8363nm, and its XRD collection of illustrative plates contrasts with reference material simultaneously, and meet very much, therefore the provable catalyst granules prepared is very pure NiO particle.
Embodiment 4: the preparation of nickel oxide/alumina catalyst
1, by the Ni (OH) of drying
2powder, γ-Al2O3 carrier and Ni (OH)
2put into crucible, send into Muffle furnace, at the temperature lower calcination 1h of 450 DEG C, then Ni (OH)
2pyrolytic makes nickel oxide powder, and load, in γ-Al2O3, becomes loaded nano nickel oxide/alumina (NiO/ γ-Al
2o
3) catalyst.
2, by the Ni (OH) of drying
2powder, γ-Al2O3 carrier and Ni (OH)
2put into crucible, send into Muffle furnace, 400 DEG C or temperature lower calcination 2h, then obtain loaded nano nickel oxide/alumina (NiO/ γ-Al
2o
3) catalyst.
3, by the Ni (OH) of drying
2powder, γ-Al2O3 carrier and Ni (OH)
2put into crucible, send into Muffle furnace, 420 DEG C or temperature lower calcination 1.5h, then obtain loaded nano nickel oxide/alumina (NiO/ γ-Al
2o
3) catalyst.
Above-mentioned surfactant can select the kinds of surface activating agents such as neopelex, and surfactant can reduce the gravitation between particle greatly, effectively can reduce the generation of particle agglomeration phenomenon.
The XRD of obtained nickel oxide/alumina catalyst is schemed as shown in Figure 5, can find that in this collection of illustrative plates 5 diffraction maximums of nickel oxide exist more clearly, prove that nickel oxide well loads on active oxidation al composition.
Embodiment 5: the application of composite nano nickel-base catalyst
1, the application process of composite nano nickel-base catalyst of the present invention: S1: dolomite is carried out calcining 18 minutes being not less than at 1000 DEG C, obtains the dolomite after calcining; S2: prepare loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst; S3: house refuse is added in pyrolysis gasification reactor; S4: by the dolomite after calcining and loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst is added in house refuse 600 DEG C at carries out pyrolysis gasification in mass ratio at 15: 75, can effectively remove the tar produced in garbage cracking process.
2, the application process of composite nano nickel-base catalyst of the present invention: S1: dolomite is carried out calcining 8 minutes being not less than at 1000 DEG C, obtains the dolomite after calcining; S2: prepare loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst; S3: house refuse is added in pyrolysis gasification reactor; S4: by the dolomite after calcining and loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst is added in house refuse 900 DEG C at carries out pyrolysis gasification in mass ratio at 15: 85, can effectively remove the tar produced in garbage cracking process.
3, the application process of composite nano nickel-base catalyst of the present invention: S1: dolomite is carried out calcining 30 minutes being not less than at 1000 DEG C, obtains the dolomite after calcining; S2: prepare loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst; S3: house refuse is added in pyrolysis gasification reactor; S4: by the dolomite after calcining and loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst is added in house refuse 800 DEG C at carries out pyrolysis gasification in mass ratio at 15: 60, can effectively remove the tar produced in garbage cracking process.
4, the application process of composite nano nickel-base catalyst of the present invention: S1: dolomite is carried out calcining 30 minutes being not less than at 1000 DEG C, obtains the dolomite after calcining; S2: prepare loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst; S3: house refuse is added in pyrolysis gasification reactor; S4: by the dolomite after calcining and loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst is added in house refuse 800 DEG C at carries out pyrolysis gasification in mass ratio at 30: 75, can effectively remove the tar produced in garbage cracking process.
At loaded nano NIO/Al
2o
3under catalyst action, carry out the experiment of domestic waste catalytic pyrolysis under 900 DEG C of temperature conditions, result shows to add loaded nano NiO/Al
2o
3after catalyst, garbage cracking factor of created gase obviously increases, and is increased to 82.37% from 70.07%; Tar yield sharply declines, and drops to about 3% from 27.98%; But the change of lime-ash productive rate is less, this illustrates that the active component nanometer NIO in catalyst serves good catalytic action, loaded nano NIO/Al to coke tar cracking reaction
2o
3the removal effect of catalyst to tar is obvious, and tar major part is converted into gas products.
Catalyst is on the impact of catalytic pyrolysis aerogenic composition: when gasification temperature increases to 900 DEG C from 750 DEG C, and after adding catalyst, catalytic gasification aerogenesis main component is H
2, CO and CH
4, compare with catalyst-free cracking, add loaded nano NIO/Al
2o
3catalyst can significantly improve H and CO content.
The existence of catalyst can change the distribution of product in pyrolysis of coal, but catalyst is on the impact of tar yield, depends on pyrolysis atmosphere to a great extent.In blanket of nitrogen, the Main Function of catalyst is micro-molecular gas material and Small molecular hydro carbons volatile matter catalytic cracking, to raising tar yield without obvious effect.In a hydrogen atmosphere, catalytic hydropyrolysis can effectively improve tar yield, because hydrogen molecule is more prone to be dissociated into hydroperoxyl radical, is conducive to house refuse and pyrolysis of coal is reacted.
The present invention is not limited to above-mentioned preferred forms, anyone for the present invention any modification done under enlightenment of the present invention or change, and every have identical with the application or akin technical scheme, all drops within protection scope of the present invention.
Claims (10)
1. a composite nano nickel-base catalyst, is characterized in that: described composite nano nickel-base catalyst comprises the dolomite after calcining and nickel-base catalyst, and the mass ratio of the two is: 15 ~ 30: 75 ~ 85; Described nickel-base catalyst is loaded nano nickel oxide/alumina catalyst.
2. a preparation method for composite nano nickel-base catalyst according to claim 1, is characterized in that: its preparation method comprises the following steps:
1. dolomite is carried out calcining 8 ~ 30 minutes being not less than at 1000 DEG C, obtain the dolomite after calcining;
2. be raw material with Nickelous nitrate hexahydrate, and add complexant, then at 180 ~ 300 DEG C, adopt Coordination homogeneous precipitation legal system for nano NiO presoma; The ratio of described Nickelous nitrate hexahydrate and ammoniacal liquor is 10.17 ~ 17.8g/100mL:
3. γ-Al2O3 carrier, nano NiO presoma and surfactant is added, 1 ~ 1.5h is calcined at 400 ~ 450 DEG C, the nano NiO presoma of load on alumina particle is decomposed into nano-nickel oxide, and then can obtain loaded nano nickel oxide/alumina catalyst;
4. by step 1. in dolomite after calcining and step 3. in the loaded nano nickel oxide/alumina catalyst mix of gained obtain described composite nano nickel-base catalyst.
3. the preparation method of composite nano nickel-base catalyst according to claim 2, is characterized in that: step 2. in Nickelous nitrate hexahydrate and the complexant temperature that is prepared nano NiO presoma be 220 ~ 260 DEG C.
4. the preparation method of composite nano nickel-base catalyst according to claim 3, is characterized in that: described complexant is ammoniacal liquor, and described ammoniacal liquor is the ammoniacal liquor after the dilution adding 3 times of volume water gagings in ammoniacal liquor.
5. the preparation method of composite nano nickel-base catalyst according to claim 4, is characterized in that: step 2. described in the ratio of Nickelous nitrate hexahydrate and ammoniacal liquor be 15 ~ 16g/100mL.
6. the preparation method of composite nano nickel-base catalyst according to claim 3, is characterized in that: described NiO presoma is nickel hydroxide.
7. the preparation method of composite nano nickel-base catalyst according to claim 3, is characterized in that: step 3. in add surfactant.
8. the preparation method of composite nano nickel-base catalyst according to claim 3, it is characterized in that: step 3. in uniform load nano-nickel oxide (NiO) on alumina support, the thickness of this nano-nickel oxide (NiO) layer is 8 ~ 500 μm.
9. the preparation method of composite nano nickel-base catalyst according to claim 1, it is characterized in that: on described alumina support, the nano-nickel oxide of load is for be made up of some nickel oxide (NiO) nanometer sheet, this nickel oxide (NiO) nanometer sheet is upright interlaced growth on the alumina support, and the thickness of this nickel oxide (NiO) nanometer sheet is 40nm-3 μm.
10. an application process for composite nano nickel-base catalyst according to claim 1, is characterized in that: described application process comprises the following steps: S1: house refuse be added in pyrolysis gasification reactor; S2: by the dolomite after calcining and loaded nano nickel oxide/alumina (NiO/Al
2o
3) catalyst is added in mass ratio in rubbish and carries out pyrolysis gasification at 600 DEG C ~ 900 DEG C, can remove the tar produced in garbage cracking process.
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Cited By (6)
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| CN104941648A (en) * | 2015-06-19 | 2015-09-30 | 东南大学 | Method for preparing nanometer Ni2O3/PG catalyst with coordination homogenizing precipitation method |
| CN105665423A (en) * | 2016-03-22 | 2016-06-15 | 北京神雾环境能源科技集团股份有限公司 | System and method for disposing household waste |
| CN106902885A (en) * | 2017-03-29 | 2017-06-30 | 中国矿业大学 | Ion-exchange prepares metal ni-loaded catalyst method and catalyst and application |
| CN107715887A (en) * | 2017-10-24 | 2018-02-23 | 江门绿润环保科技有限公司 | A kind of preparation method and applications of the nickel-base catalyst of modification dolomite load |
| CN110261191A (en) * | 2019-05-23 | 2019-09-20 | 中国石油天然气股份有限公司 | A kind of method of bonding state biomarker in extraction hydrocarbon source rock |
| CN110491599A (en) * | 2019-08-05 | 2019-11-22 | 重庆文理学院 | A kind of preparation method of composite conductive thin film |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104941648A (en) * | 2015-06-19 | 2015-09-30 | 东南大学 | Method for preparing nanometer Ni2O3/PG catalyst with coordination homogenizing precipitation method |
| CN105665423A (en) * | 2016-03-22 | 2016-06-15 | 北京神雾环境能源科技集团股份有限公司 | System and method for disposing household waste |
| CN106902885A (en) * | 2017-03-29 | 2017-06-30 | 中国矿业大学 | Ion-exchange prepares metal ni-loaded catalyst method and catalyst and application |
| CN106902885B (en) * | 2017-03-29 | 2019-08-13 | 中国矿业大学 | Ion-exchange prepares metal ni-loaded catalyst method and catalyst and application |
| CN107715887A (en) * | 2017-10-24 | 2018-02-23 | 江门绿润环保科技有限公司 | A kind of preparation method and applications of the nickel-base catalyst of modification dolomite load |
| CN110261191A (en) * | 2019-05-23 | 2019-09-20 | 中国石油天然气股份有限公司 | A kind of method of bonding state biomarker in extraction hydrocarbon source rock |
| CN110261191B (en) * | 2019-05-23 | 2021-11-02 | 中国石油天然气股份有限公司 | Method for extracting bonded-state biomarker in hydrocarbon source rock |
| CN110491599A (en) * | 2019-08-05 | 2019-11-22 | 重庆文理学院 | A kind of preparation method of composite conductive thin film |
| CN110491599B (en) * | 2019-08-05 | 2021-09-03 | 重庆文理学院 | Preparation method of composite conductive film |
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