CN109999626A - A method of preparing copper oxide/carbon nano-fiber flexible compound gas desulfurizer - Google Patents
A method of preparing copper oxide/carbon nano-fiber flexible compound gas desulfurizer Download PDFInfo
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- CN109999626A CN109999626A CN201910358135.8A CN201910358135A CN109999626A CN 109999626 A CN109999626 A CN 109999626A CN 201910358135 A CN201910358135 A CN 201910358135A CN 109999626 A CN109999626 A CN 109999626A
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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
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
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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
- B01D53/81—Solid phase processes
Abstract
The invention belongs to coal chemical industry technical field of desulfurizer preparation, a kind of preparation method of copper oxide/carbon nano-fiber flexible compound gas desulfurizer, the dissolution in solvent n,N-Dimethylformamide (DMF) by polyacrylonitrile, and cupric oxalate is mixed as active component CuO presoma with polymer solution；It is synthesized using electrostatic spinning technique by cupric oxalate/polyacrylonitrile fibre composite material；Finally composite material can be obtained by microwave high-temperature annealing.Inventive desulfurization material technology route is simple, easy to implement, can satisfy the industrialized performance requirement of desulfurizing agent；On the other hand, desulfurizing agent constructs desulfurizing agent multistage micropore structure as carrier using flexibility height, porosity polymer fiber abundant, and the adsorption capacity and desulphurization reaction activity of desulfurizing agent can be improved.
Description
Technical field
The invention belongs to coal chemical industry technical field of desulfurizer preparation, are related to a kind of preparation method of gas desulfurizer.
Background technique
As the coal of one of the three macrofossil energy, the critical role of basic energy resource can not in the economic development in China
Shake, but various environmental problems caused by directly being burnt by coal have to attract people's attention.Integral coal gasification connection
Conjunction power generation technology (IGCC) is based on the clean and effective utilization to coal, is shown on a large scale by many countries and regions
Model.Coal gas is as the power and raw material sources in IGCC technology, containing a large amount of sulfide, wherein 90% the above are stink damps
Body.Hydrogen sulfide can not only cause burn into make catalyst poisoning industrial equipment, and being discharged into after atmosphere can also be to ecological environment and human body
Health threatens.It therefore, must be clean by hydrogen sulfide stripping therein before coal gas uses.
Dry desulfurization by the metal oxide in solid phase desulfurizing agent in the way of chemically reacting by H2S conversion removing, should
The advantages that method has process flow simple, no waste water, waste acid treatment problem, low energy consumption, small to equipment corrosion, at low cost.
Early in 1976, Westmoreland et al. has been filtered out in the periodic table of elements can be living as gas desulfurizer metal oxide
Element (Fe, Zn, Mn, Mo, V, Ca, Si, Ba, Co, Cu, W) in the 11 of property component.Studies have shown that using zinc oxide as active component
Desulfurizing agent possess higher desulfurization precision and desulfuration efficiency than other oxide desulfurizing agents, but zinc oxide is in high temperature regeneration mistake
It is volatile in journey, lead to loss of active component, performance decline is serious.Between copper oxide and hydrogen sulfide have very strong affinity and
Adsorption capacity.There is scholar to find copper oxide desulfurizing agent desulfurization precision with higher, be affected by temperature smaller and have good
Regenerability.
In gas desulfurizer reaction process, since sulfur product metal sulfide occupies bigger sky than metal oxide
Between, cause to be easy to cause desulfurizing agent internal volume to expand because of the displacement of oxygen sulphur as the desulfurizing agent of carrier using conventional rigid material, cause
Internal structure is collapsed and pore plugging, larger to the diffusion limitation of reaction rate, microcosmic mass transfer and ion, this has seriously affected desulfurization
Agent it is desulphurizing activated.Therefore, optimizing the texture property of desulfurizing agent and improving active component occurrence status is to improve metal oxide
The important directions that desulfurizing agent efficiently utilizes.
Existing patent CN201510626135.3, CN201610332695.2 and CN200810041467.5 are individually disclosed
The different preparation method of copper oxide desulfurizing agent.Although above method technology maturation, there are energy consumptions, and the environment such as high, seriously polluted are asked
Topic.Even more there are Active components distributions for some desulfurizing agents unevenly, specific surface area and hole are held relatively small, pore structure and not enough sent out
Up to the problems such as, cause the desulfurization performance of prepared desulfurizing agent unsatisfactory, it is difficult to reach industrial requirement.
Summary of the invention
Copper oxide/carbon nano-fiber flexible compound gas desulfurizer method is prepared the object of the present invention is to provide a kind of,
To solve, porosity during reactive desulfurizing agent, active component utilization rate are low and desulfurizing agent vulcanization-regenerability difference is asked
Topic, and finally improve the curability of desulfurizing agent.
The technical scheme adopted by the invention is that: a kind of system of copper oxide/carbon nano-fiber flexible compound gas desulfurizer
Preparation Method includes the following steps:
(1) polyacrylonitrile (PAN) powder is added to stirring and dissolving in n,N-Dimethylformamide solution, then by active component
CuO presoma cupric oxalate CuC2O4It is added to and continues to stir evenly to form mixed solution in polymer solution, this three's mass percentage
Than composition, PAN accounts for three gross mass 5.5-11.3%, and n,N-Dimethylformamide accounts for three gross mass 69.5-86.9%,
CuC2O4 Account for three's gross mass 7.6-19.2%；
(2) to mixed solution by electrostatic spinning synthesis of oxalic acid copper/polyacrylonitrile fibre composite material, electrostatic spinning process is in work
Skill condition is voltage 9-17 V, 20-40 DEG C of environment temperature, ambient humidity 15-75%, propulsive liquid speed 1-3mL/min, reception device
For spinning 2-6h under roller and its revolving speed 50-90r/min, reception distance 5-25cm；(3) after drying by composite material in 80-
It is dried at 100 DEG C, finally at 180-260 DEG C in such a way that microwave high-temperature anneals (microwave radiation of power 300-800W)
1-3 h is pre-oxidized under air atmosphere, that CuO/CNFs flexibility can be obtained is multiple by high temperature cabonization 3-5 h under 600-800 DEG C of nitrogen atmosphere
Close gas desulfurizer.
In prepared CuO/CNFs flexible compound gas desulfurizer, mass percentage composition is CuO 5-25%.
The fibre diameter of the carbon nano-fiber materials is 0.1-1 μm, surface density 1-20g/m2。
The beneficial effects of the present invention are: desulfurizing agent uses carbon nano-fiber CNFs for carrier in (1) present invention, it is being active
While component provides bracket effect, carbon nano-fiber pore structure abundant can promote desulfurizing agent absorption and reaction process
It carries out.In addition, carbon nano-fiber has excellent mechanical property and flexibility, has the flexibility of multi-level, multistage confinement hole
Structure can be avoided desulfurization product volume and increase the spalling of bring pore structure, eliminates or weakens in reaction process in desulfurizing agent
The adverse effect that portion's microstructure expansion-contraction generates, optimization texture, restricted activity component is mobile and then reduces its aggregation, fills
The nano effect of material is waved in distribution, realizes the reinforcing of gas-solid reaction rate and mass-transfer efficiency, reduces desulfurizing agent structural behaviour drop
It is low, improve the desulfuration efficiency of unit desulfurizing agent.(2) desulfurizing agent preparation method process route is simple in the present invention, implementation cost
Low, industrialization promotion is easy, and can satisfy the wilderness demand in market.(3) using microwave radiation as desulfurizing agent high annealing mistake
Chemical reaction efficiency can be improved in heat source in journey, the time required to shortening reaction, reduces the time cost of desulfurizing agent preparation.Through
Test, copper oxide/carbon nano-fiber flexible compound gas desulfurizer that through the invention prepared by middle method, not only single Sulfur capacity is protected
It holds 15% or more, and after ten vulcanizations-regeneration cycle use, still there is 99% Sulfur capacity conservation rate.
Specific embodiment
Following embodiments are only the preferred technical solution of the present invention, are not used to carry out any restrictions to the present invention.For
For those skilled in the art, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made
Any modification, equivalent substitution, improvement and etc., should all be included in the protection scope of the present invention.
Comparative example 1.
Pure zinc oxide desulfurizing agent is prepared using conventional method, and CuO/ will be prepared after the simple and mechanical mixing of CuO and CNFs
CNFs desulfurizing agent.Wherein, the active component content of the CuO/CNFs desulfurizing agent of mechanical mixture and 1 desulfurizing agent of embodiment, physical property, at
Shape parameter is consistent.
Under same desulphurization reaction experiment condition, test pure zirconia copper desulfurizing agent and mechanical mixture CuO/CNFs desulfurizing agent just
Sulfur capacity is respectively 3.3% and 8.2%.
After also passing through ten vulcanization/regeneration cycles, pure zirconia copper desulfurizing agent and mechanical mixture CuO/CNFs desulfurizing agent
Sulfur capacity falls to 1.6% and 5.3% respectively.
Embodiment 1.
Polyacrylonitrile (PAN) powder 1g is added to stirring and dissolving in 15.67g n,N-Dimethylformamide solution, then
By 1.36g active component CuO presoma cupric oxalate (CuC2O4) be added to and continue to stir evenly in polymer solution；Using routine
Electrospinning device passes through electrostatic spinning synthesis of oxalic acid copper/polypropylene to mixed solution using method generally in the art later
Nitrile fibrous composite (don't explain too much here), electrostatic spinning process are 9 V of voltage, environment temperature 20 in process conditions
DEG C, ambient humidity 15%, propulsive liquid speed be 1.0mL/min, reception device is roller and its revolving speed is 50r/min, receives distance
For spinning 2h under 5cm；Composite material can be obtained into CuO/CNFs gas desulfurizer, institute with microwave high-temperature annealing after drying
State the dry progress at 80 DEG C of desulfurizing agent, microwave high-temperature annealing pre-oxidizes 1h, 600 DEG C of nitrogen atmospheres under 180 DEG C of air atmospheres
CuO/CNFs gas desulfurizer can be obtained in lower high temperature cabonization 3h.
CuO/CNFs gas desulfurizer prepared by embodiment 1 is placed in fixed-bed reactor, with 2000 h of air speed-1It is logical
Enter Texaco's simulation coal gas, desulphurization reaction is carried out at 500 DEG C.
After desulfurization, the Sulfur capacity for detecting desulfurizing agent has reached 15.26%.
And then the secondary mixing air using oxygen volumetric concentration 2%, at 650 DEG C of temperature, 2000 h of air speed-1Under, to de-
After sulphur agent is regenerated, continue on for carrying out in the desulphurization reaction of Texaco's simulation coal gas.
So after ten vulcanizations/regeneration cycle use, the Sulfur capacity for detecting desulfurizing agent is 15.11%.
By the comparison of embodiment 1 and comparative example 1 as can be seen that the CuO/CNFs prepared using heretofore described method
Sulfur capacity after desulfurizing agent single Sulfur capacity and ten circulations is far higher by conventional method and prepares the corresponding Sulfur capacity of desulfurizing agent.
Embodiment 2.
Polyacrylonitrile (PAN) powder 1g is added to stirring and dissolving in 11.50g n,N-Dimethylformamide solution, then
By 1.43g active component CuO presoma cupric oxalate (CuC2O4) be added to and continue to stir evenly in polymer solution；Using routine
Electrospinning device passes through electrostatic spinning synthesis of oxalic acid copper/polypropylene to mixed solution using method generally in the art later
Nitrile fibrous composite (don't explain too much here), electrostatic spinning process process conditions be voltage 11V, environment temperature 25
DEG C, ambient humidity 30%, propulsive liquid speed be 1.5mL/min, reception device is roller and its revolving speed is 60r/min, receives distance
For spinning 3h under 10cm；Composite material can be obtained into CuO/CNFs gas desulfurizer with microwave high-temperature annealing after drying,
The dry progress at 85 DEG C of the desulfurizing agent, microwave high-temperature annealing pre-oxidize 1.5h, 650 DEG C of nitrogen under 200 DEG C of air atmospheres
CuO/CNFs gas desulfurizer can be obtained in high temperature cabonization 3.5h under atmosphere.
CuO/CNFs gas desulfurizer prepared by embodiment 2 is placed in fixed-bed reactor, with 2000 h of air speed-1It is logical
Enter Texaco's simulation coal gas, desulphurization reaction is carried out at 500 DEG C.
After desulfurization, the Sulfur capacity for detecting desulfurizing agent has reached 15.57%.
And then the secondary mixing air using oxygen volumetric concentration 2%, at 650 DEG C of temperature, 2000 h of air speed-1Under, to de-
After sulphur agent is regenerated, continue on for carrying out in the desulphurization reaction of Texaco's simulation coal gas.
So after ten vulcanizations/regeneration cycle use, the Sulfur capacity for detecting desulfurizing agent is 15.33%.
Embodiment 3.
Polyacrylonitrile (PAN) powder 1g is added to stirring and dissolving in 9.00g n,N-Dimethylformamide solution, then
By 1.51g active component CuO presoma cupric oxalate (CuC2O4) be added to and continue to stir evenly in polymer solution；Using routine
Electrospinning device passes through electrostatic spinning synthesis of oxalic acid copper/polypropylene to mixed solution using method generally in the art later
Nitrile fibrous composite (don't explain too much here), electrostatic spinning process process conditions be voltage 13V, environment temperature 30
DEG C, ambient humidity 45%, propulsive liquid speed be 2.0mL/min, reception device is roller and its revolving speed is 70r/min, receives distance
For spinning 4h under 15cm；Composite material can be obtained into CuO/CNFs gas desulfurizer with microwave high-temperature annealing after drying,
The dry progress at 90 DEG C of the desulfurizing agent, microwave high-temperature annealing pre-oxidize 2h, 700 DEG C of nitrogen gas under 220 DEG C of air atmospheres
CuO/CNFs gas desulfurizer can be obtained in high temperature cabonization 4h under atmosphere.
CuO/CNFs gas desulfurizer prepared by embodiment 3 is placed in fixed-bed reactor, with 2000 h of air speed-1It is logical
Enter Texaco's simulation coal gas, desulphurization reaction is carried out at 500 DEG C.
After desulfurization, the Sulfur capacity for detecting desulfurizing agent has reached 15.89%.
And then the secondary mixing air using oxygen volumetric concentration 2%, at 650 DEG C of temperature, 2000 h of air speed-1Under, to de-
After sulphur agent is regenerated, continue on for carrying out in the desulphurization reaction of Texaco's simulation coal gas.
So after ten vulcanizations/regeneration cycle use, the Sulfur capacity for detecting desulfurizing agent is 15.65%.
Embodiment 4.
Polyacrylonitrile (PAN) powder 1g is added to stirring and dissolving in 7.33g n,N-Dimethylformamide solution, then
By 1.60g active component CuO presoma cupric oxalate (CuC2O4) be added to and continue to stir evenly in polymer solution；Using routine
Electrospinning device passes through electrostatic spinning synthesis of oxalic acid copper/polypropylene to mixed solution using method generally in the art later
Nitrile fibrous composite (don't explain too much here), electrostatic spinning process process conditions be voltage 15V, environment temperature 35
DEG C, ambient humidity 60%, propulsive liquid speed be 2.5mL/min, reception device is roller and its revolving speed is 80r/min, receives distance
For spinning 5h under 20cm；Composite material can be obtained into CuO/CNFs gas desulfurizer with microwave high-temperature annealing after drying,
The dry progress at 95 DEG C of the desulfurizing agent, microwave high-temperature annealing pre-oxidize 2.5h, 750 DEG C of nitrogen under 240 DEG C of air atmospheres
CuO/CNFs gas desulfurizer can be obtained in high temperature cabonization 4.5h under atmosphere.
CuO/CNFs gas desulfurizer prepared by embodiment 4 is placed in fixed-bed reactor, with 2000 h of air speed-1It is logical
Enter Texaco's simulation coal gas, desulphurization reaction is carried out at 500 DEG C.
After desulfurization, the Sulfur capacity for detecting desulfurizing agent has reached 16.26%.
And then the secondary mixing air using oxygen volumetric concentration 2%, at 650 DEG C of temperature, 2000 h of air speed-1Under, to de-
After sulphur agent is regenerated, continue on for carrying out in the desulphurization reaction of Texaco's simulation coal gas.
So after ten vulcanizations/regeneration cycle use, the Sulfur capacity for detecting desulfurizing agent is 16.08%.
Embodiment 5.
Polyacrylonitrile (PAN) powder 1g is added to stirring and dissolving in 6.14g n,N-Dimethylformamide solution, then
By 1.70g active component CuO presoma cupric oxalate (CuC2O4) be added to and continue to stir evenly in polymer solution；Using routine
Electrospinning device passes through electrostatic spinning synthesis of oxalic acid copper/polypropylene to mixed solution using method generally in the art later
Nitrile fibrous composite (don't explain too much here), electrostatic spinning process process conditions be voltage 17V, environment temperature 40
DEG C, ambient humidity 75%, propulsive liquid speed be 3.0mL/min, reception device is roller and its revolving speed is 90r/min, receives distance
For spinning 6h under 25cm；Composite material can be obtained into CuO/CNFs gas desulfurizer with microwave high-temperature annealing after drying,
The dry progress at 95 DEG C of the desulfurizing agent, microwave high-temperature annealing pre-oxidize 3h, 800 DEG C of nitrogen gas under 260 DEG C of air atmospheres
CuO/CNFs gas desulfurizer can be obtained in high temperature cabonization 5h under atmosphere.
CuO/CNFs gas desulfurizer prepared by embodiment 5 is placed in fixed-bed reactor, with 2000 h of air speed-1It is logical
Enter Texaco's simulation coal gas, desulphurization reaction is carried out at 500 DEG C.
After desulfurization, the Sulfur capacity for detecting desulfurizing agent has reached 16.11%.
And then the secondary mixing air using oxygen volumetric concentration 2%, at 650 DEG C of temperature, 2000 h of air speed-1Under, to de-
After sulphur agent is regenerated, continue on for carrying out in the desulphurization reaction of Texaco's simulation coal gas.
So after ten vulcanizations/regeneration cycle use, the Sulfur capacity for detecting desulfurizing agent is 15.97%.
Claims (3)
1. a kind of copper oxide/carbon nano-fiber flexible compound gas desulfurizer preparation method, it is characterised in that: including walking as follows
It is rapid:
(1) polyacrylonitrile (PAN) powder is added to stirring and dissolving in n,N-Dimethylformamide solution, then by active component
CuO presoma cupric oxalate CuC2O4It is added to and continues to stir evenly to form mixed solution in polymer solution, this three's mass percentage
Than composition, PAN accounts for three gross mass 5.5-11.3%, and n,N-Dimethylformamide accounts for three gross mass 69.5-86.9%,
CuC2O4 Account for three's gross mass 7.6-19.2%；
(2) to mixed solution by electrostatic spinning synthesis of oxalic acid copper/polyacrylonitrile fibre composite material, electrostatic spinning process is in work
Skill condition is voltage 9-17 V, 20-40 DEG C of environment temperature, ambient humidity 15-75%, propulsive liquid speed 1-3mL/min, reception device
For spinning 2-6h under roller and its revolving speed 50-90r/min, reception distance 5-25cm；(3) after drying by composite material in 80-
Be dried at 100 DEG C, finally by microwave high-temperature annealing in a manner of under 180-260 DEG C of air atmosphere pre-oxidize 1-3 h,
CuO/CNFs flexible compound gas desulfurizer can be obtained in high temperature cabonization 3-5 h under 600-800 DEG C of nitrogen atmosphere.
2. a kind of copper oxide/carbon nano-fiber flexible compound gas desulfurizer preparation method according to claim 1, special
Sign is: in prepared CuO/CNFs flexible compound gas desulfurizer, mass percentage composition is CuO 5-25%.
3. a kind of copper oxide/carbon nano-fiber flexible compound gas desulfurizer preparation method according to claim 1, special
Sign is: the fibre diameter of the carbon nano-fiber materials is 0.1-1 μm, surface density 1-20g/m2。
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| CN111763540A (en) * | 2020-06-08 | 2020-10-13 | 太原理工大学 | Preparation method of zinc oxide gas desulfurizer |
| CN113893878A (en) * | 2021-10-15 | 2022-01-07 | 海南师范大学 | Preparation method and application of nanofiber-supported heteropolyacid salt catalyst |
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| CN117181306A (en) * | 2023-11-07 | 2023-12-08 | 明硕环境科技集团股份有限公司 | Preparation method of hydrolysis desulfurization bifunctional catalyst for blast furnace gas |
| CN117181306B (en) * | 2023-11-07 | 2024-03-15 | 明硕环境科技集团股份有限公司 | Preparation method of hydrolysis desulfurization bifunctional catalyst for blast furnace gas |
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