CN109225234A - A kind of composition for carbon catalytic hydrogenation methane - Google Patents
A kind of composition for carbon catalytic hydrogenation methane Download PDFInfo
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- CN109225234A CN109225234A CN201811083967.5A CN201811083967A CN109225234A CN 109225234 A CN109225234 A CN 109225234A CN 201811083967 A CN201811083967 A CN 201811083967A CN 109225234 A CN109225234 A CN 109225234A
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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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/18—Reducing with gases containing free hydrogen
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- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
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Abstract
The invention discloses a kind of composition for carbon catalytic hydrogenation methane, the component of the composition includes: cobalt salt, molysite and calcium salt, wherein Co: Fe: Ca mass ratio is 0.25~1.5: 0.25~1.5: 1.5.Compared with the catalyst of existing coal catalytic hydrogenation methane, composition of the invention uses Co-Fe-Ca triple combination, not only has good catalytic effect, but also has the advantages that stability is good, not easy in inactivation, at low cost, is suitable for being industrially used.
Description
Technical field
The invention belongs to catalytic hydrogenation fields, and in particular to a kind of composition for carbon catalytic hydrogenation methane, and
Application of the composition in solid carbon-contg material catalytic hydrogenation methane.
Background technique
The total energy characteristics in China are " more coals, oil-poor, few gas ", with China's expanding economy and environmental protection plus
By force, the demand of natural gas rises rapidly, and it is suitable state of China that the coal of rich reserves, which is converted to natural gas by catalytic gasification,
The selection of feelings and development strategy and resource high-efficiency integration and the inexorable trend for improving coal resources utilization rate.
According to the difference of chemical reaction step, coal natural gas technology can be divided into direct natural gas from coal technology and indirect coal
Natural gas technology processed.Indirect coal natural gas technology is then to carry out synthesis gas methanation by synthesis gas is made in coal gasification.With
It connects coal natural gas to compare, the main reaction of direct natural gas from coal technology is C+2H2→CH4, have process it is short, simple process and
Feature with low investment.
The catalyst of the existing direct catalytic hydrogenation methane of coal is mostly alkali metal sylvite and sodium salt and transition metal such as cobalt
Salt nickel salt.Wherein the catalytic effect of alkali metal especially potassium carbonate is best, still, negative due to alkali metal using also most extensively
Carrying capacity is big, good fluidity be easy be lost, easily cause equipment to corrode, also be easy with minerals in coal ining conjunction with generation alumino-silicate thus
Lead to catalyst inactivation.Cobalt Raney nickel also has preferable catalytic effect, but price is higher, as cobalt price 45~550,000 yuan/
Ton, nickel price 10~150,000 yuan/ton, fancy price cause cobalt Raney nickel at high cost, it is difficult to realize industrialization.
Patent document CN106311339A discloses one kind for coal hydrogenation catalytic gasification catalyst, which includes 1-
The nickel salt and/or molysite of 5wt%, one or more of soluble calcium salt, magnesium salts, manganese salt and zinc salt of 1-5wt%, 1-
The Organic Sodium Salt and/or sylvite of 15wt%, remaining ingredient are mainly the coal sill of 40-80 mesh.The catalyst can not be from root
Traditional base metal catalysts are solved the disadvantage that in sheet.
Therefore, there is excellent catalytic gasification performance there is an urgent need to one kind and stability is good, not easy in inactivation, economic cost ratio
Lower catalyst is applied to industrialization.
Summary of the invention
Problem mentioned in the background art, that it is an object of the invention to a kind of stability is good, not easy in inactivation, at low cost
Composition and the composition the answering in solid carbon-contg material catalytic hydrogenation methane for carbon catalytic hydrogenation methane
With.
To achieve the above object, the invention provides the following technical scheme:
A kind of composition for carbon catalytic hydrogenation methane, the component of the composition include: cobalt salt, molysite and calcium
Salt, wherein Co: Fe: Ca mass ratio is 0.25~1.5: 0.25~1.5: 1.5.
Preferably, Co: Fe: Ca mass ratio is 1~1.25: 0.25~0.5: 1.5.
Preferably, the cobalt salt is cobalt nitrate, and the molysite is ferric nitrate, and the calcium salt is calcium nitrate.
Above-mentioned composition reacts generation methane with hydrogen for being catalyzed carbon, such as in solid carbon-contg material catalytic hydrogenation methane
In main reaction: C+2H2→CH4。
A kind of method of solid carbon-contg material catalytic hydrogenation methane, comprising:
(1) combinations of the above object is mixed with solid carbon-contg material, obtains mixture;
(2) mixture that step (1) obtains is reacted in hydrogenator with hydrogen, obtains methane.
It preferably, is the solid carbon-contg quality of material by the total amount of Co, Fe, Ca in the composition in step (1)
1~6%, the composition is mixed with the solid carbon-contg material, it is highly preferred that in the composition Co, Fe, Ca total amount
It is the 3~4% of the solid carbon-contg quality of material.
Preferably, step (1), the composition are mixed with the solid carbon-contg material using infusion process: by the combination
Object first uses aqueous solution, adds the solid carbon-contg material, impregnates, dry.It is mixed using infusion process, composition can be made more preferable
Ground is dispersed in the surface of solid carbon-contg material.
Preferably, in step (2), the temperature of the reaction is 700~850 DEG C, and Hydrogen Vapor Pressure is normal pressure to 6MPa;It is preferred that
Ground, the temperature of the reaction are 750 DEG C, Hydrogen Vapor Pressure 2MPa.
Preferably, the solid carbon-contg material is coal or coal tar.
Beneficial effect
1, composition of the invention uses Co-Fe-Ca triple combination, has to solid carbon-contg material catalytic hydrogenation methane
Good catalytic effect, and synergistic effect can be generated between Co-Fe-Ca three.
2, composition of the invention can overcome existing alkali metal series catalysts load capacity big, and good fluidity is easy to be lost,
It easily causes equipment to corrode, is also easy to generate the shortcomings that alumino-silicate is so as to cause catalyst inactivation in conjunction with minerals in coal.
3, composition of the invention substitutes the Co of part with Fe, can reduce cost.
Specific embodiment
The technical solution in the content of present invention will be clearly and completely described below, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The coal of coal tar used in the embodiment of the present invention is Yi Li lignite.
Embodiment 1
Weigh the Co (NO of 0.0617g3)2·6H20, the Fe (NO of 0.0181g3)3·9H2O, the Ca (NO of 0.0884g3)2·
4H2O is uniformly mixed and is placed in small beaker, and mixed solution is uniformly made in the deionized water ultrasound that 0.7ml is added.By 1g coal tar (20
~60 mesh) it is add to the above mixed solution, after ultrasonic immersing 2 hours, it is put into 105 DEG C of air dry oven drying 24 hours,
It is cooled to room temperature and is put into drier and save backup.
Fixed bed reactors will be added through treated coal tar, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of gas velocity 50ml/min, and product methane is made.
Embodiment 2
Weigh the Co (NO of 0.0496g3)2·6H2O, the Fe (NO of 0.0362g3)3·9H2O, the Ca (NO of 0.0884g3)2·
4H2O mixing is placed in small beaker, and mixed solution is uniformly made in the deionized water ultrasound that 0.7ml is added.By 1g coal tar (20~60 mesh)
It is add to the above mixed solution, after ultrasonic immersing 2 hours, is put into 105 DEG C of air dry oven drying 24 hours, is cooled to
Room temperature is put into drier and saves backup.
Fixed bed reactors will be added through treated coal tar, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of gas velocity 50ml/min, and product methane is made.
Embodiment 3
Weigh the Co (NO of 0.0372g3)2·6H2O, the Fe (NO of 0.0543g3)3·9H2O, 0.0884 Ca (NO3)2·
4H2O mixing is placed in small beaker, and mixed solution is uniformly made in the deionized water ultrasound that 0.7ml is added.By 1g coal tar (20~60 mesh)
It is add to the above mixed solution, after ultrasonic immersing 2 hours, is put into 105 DEG C of air dry oven drying 24 hours, is cooled to
Room temperature is put into drier and saves backup.
Fixed bed reactors will be added through treated coal tar, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of gas velocity 50ml/min, and product methane is made.
Embodiment 4
Weigh the Co (NO of 0.0247g3)2·6H2O, the Fe (NO of 0.0724g3)3·9H2O, the Ca (NO of 0.0884g3)2·
4H2O mixing is placed in small beaker, and mixed solution is uniformly made in the deionized water ultrasound that 0.7ml is added.By 1g coal tar (20~60 mesh)
It is add to the above mixed solution, after ultrasonic immersing 2 hours, is put into 105 DEG C of air dry oven drying 24 hours, is cooled to
Room temperature is put into drier and saves backup.
Fixed bed reactors will be added through treated coal tar, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of gas velocity 50ml/min, and product methane is made.
Embodiment 5
Weigh the Co (NO of 0.0124g3)2·6H2O, the Fe (NO of 0.0905g3)3·9H2O, the Ca (NO of 0.0884g3)2·
4H2O mixing is placed in small beaker, and mixed solution is uniformly made in the deionized water ultrasound that 0.7ml is added.By 1g coal tar (20~60 mesh)
It is add to the above mixed solution, after ultrasonic immersing 2 hours, is put into 105 DEG C of air dry oven drying 24 hours, is cooled to
Room temperature is put into drier and saves backup.
Fixed bed reactors will be added through treated coal tar, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of gas velocity 50ml/min, and product methane is made
Comparative example 1
Weigh the Co (NO of 0.0741g3)2·6H2O, the Ca (NO of 0.0884g3)2·4H2O mixing is placed in small beaker, is added
Mixed solution is uniformly made in the deionized water ultrasound of 0.7ml.1g coal tar (20~60 mesh) is add to the above mixed solution, is surpassed
After sound impregnates 2 hours, it is put into 105 DEG C of air dry oven dry 24 hours, is cooled to room temperature and is put into drier and save backup.
Fixed bed reactors will be added through treated coal tar, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of gas velocity 50ml/min, and product methane is made.
Comparative example 2
Weigh the Fe (NO of 0.1081g3)3·9H2O, the Ca (NO of 0.0884g3)2·4H2O mixing is placed in small beaker, is added
Mixed solution is uniformly made in the deionized water ultrasound of 0.7ml.1g coal tar (20~60 mesh) is add to the above mixed solution, is surpassed
After sound impregnates 2 hours, it is put into 105 DEG C of air dry oven dry 24 hours, is cooled to room temperature and is put into drier and save backup.
Fixed bed reactors will be added through treated coal tar, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of gas velocity 50ml/min, and product methane is made.
Comparative example 3
The drying box for taking 20~60 mesh coal tar 1g to be put into 105 DEG C is 24 hours dry, is cooled to room temperature and is put into drier guarantor
It deposits spare.
Fixed bed reactors are added in coal tar after above-mentioned drying, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of flow velocity 50ml/min, and product methane is made.
Comparative example 4
Weigh the Co (NO of 0.0741g3)2·6H2O is placed in small beaker, and the deionized water ultrasound that 0.7ml is added uniformly is made
Mixed solution weighs 20~60 mesh coal tar 1g and mixed solution is added, and after ultrasonic immersing 2 hours, it is dry to be put into 105 DEG C of drying box
It 24 hours, is cooled to room temperature and is put into drier and save backup.
Fixed bed reactors will be added through treated coal tar, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of gas velocity 50ml/min, and product methane is made.
Comparative example 5
Weigh the Fe (NO of 0.1081g3)3·9H2O is placed in small beaker, and the deionized water ultrasound that 0.7ml is added uniformly is made
Mixed solution weighs 20~60 mesh coal tar 1g and mixed solution is added, and after ultrasonic immersing 2 hours, it is dry to be put into 105 DEG C of drying box
It 24 hours, is cooled to room temperature and is put into drier and save backup.
Fixed bed reactors will be added through treated coal tar, in 750 DEG C of reaction temperature, Hydrogen Vapor Pressure 2MPa, hydrogen
Gasification reaction is carried out under conditions of gas velocity 50ml/min, and product methane is made.
The methane interpretation of result of Examples 1 to 5 and the Comparative Examples 1 to 5 is shown in Table 1
1 methane interpretation of result of table
According to above-described embodiment 1-5's as a result, the present invention using Co-Fe-Ca three-way catalyst to coal catalytic hydrogenation first
Alkane has good catalytic action.The mass ratio for working as Co: Fe: Ca it can be seen from the result of embodiment 1-2 and comparative example 1 is 1
When~1.25: 0.25~0.5: 1.5, the catalytic effect after part Co is substituted with Fe is suitable with the Co-Ca of same amount, this is advantageous
In reducing cost in the case where not influencing catalytic effect.
While specific embodiments of the present invention have been shown and described, but protection scope of the present invention is not limited to
This, anyone skilled in the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement
, every other embodiment obtained under the premise of creative work is not made, should all be covered in protection scope of the present invention
Within.
Claims (10)
1. a kind of composition for carbon catalytic hydrogenation methane, the component of the composition includes: cobalt salt, molysite and calcium salt,
Wherein, Co: Fe: Ca mass ratio is 0.25~1.5: 0.25~1.5: 1.5.
2. composition according to claim 1, it is characterised in that: Co: Fe: Ca mass ratio be 1~1.25: 0.25~
0.5∶1.5。
3. composition according to claim 1 or 2, it is characterised in that: the cobalt salt is cobalt nitrate, and the molysite is nitric acid
Iron, the calcium salt are calcium nitrate.
4. the purposes of any composition of claims 1 to 3, it is characterised in that: the composition is for being catalyzed carbon and hydrogen
Solid/liquid/gas reactions generate methane.
5. purposes according to claim 4, it is characterised in that: the composition is in solid carbon-contg material catalytic hydrogenation first
Application in alkane.
6. a kind of method of solid carbon-contg material catalytic hydrogenation methane, comprising:
(1) any composition of claims 1 to 3 is mixed with solid carbon-contg material, obtains mixture;
(2) mixture that step (1) obtains is reacted in hydrogenator with hydrogen, obtains methane.
7. according to the method described in claim 6, it is characterized by: in step (1), by the composition Co, Fe, Ca it is total
Amount is the 1~6% of the solid carbon-contg quality of material, the composition is mixed with the solid carbon-contg material, it is preferable that institute
The total amount for stating Co, Fe, Ca in composition is the 3~4% of the solid carbon-contg quality of material.
8. according to the method described in claim 6, it is characterized by: step (1), the composition and the solid carbon-contg material
It is mixed using infusion process.
9. according to the method described in claim 6, it is characterized by: the temperature of the reaction is 700~850 in step (2)
DEG C, Hydrogen Vapor Pressure is normal pressure to 6MPa;Preferably, the temperature of the reaction is 750 DEG C, Hydrogen Vapor Pressure 2MPa.
10. according to any method of claim 6~9, it is characterised in that: the solid carbon-contg material is coal or coal tar.
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