CN106311142A - Preparation method of carbon aerogel desulfurizer for high-temperature desulfuration - Google Patents
Preparation method of carbon aerogel desulfurizer for high-temperature desulfuration Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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Abstract
The invention discloses a preparation method of carbon aerogel desulfurizer for high-temperature desulfuration. The carbon aerogel desulfurizer for high-temperature desulfuration is prepared by applying a sol-gel method, performing sol-gel reaction under a water bath in the de-ionized water solvent by taking methanol and resorcinol as the raw material and anhydrous sodium carbonate as alkali catalyst, performing the organic solvent replacement and sealing type freeze drying on solvent, finally obtaining carbon aerogel through high-temperature carbonizing, and then orderly performing manganous nitrate immersion, drying, and forging on the carbon aerogel. The carbon aerogel desulfurizer for high-temperature desulfuration has big penetrating sulfur capacity and saturated sulfur capacity, and can be applied to the high-temperature removal process of H2S in an overall coal gasification combined cycle power generation system; moreover, the carbon aerogel desulfurizer for high-temperature desulfuration is featured by being gentle in preparation condition, regular in production equipment, and suitable for scale production, and so on.
Description
Technical field
The invention belongs to chemical field, relate to a kind of H2S desulfurizing agent, a kind of charcoal gas for high temperature desulfurizing
The preparation method of gel desulfurizing agent.
Background technology
At present, present in the coal utilization of China, subject matter is that utilization ratio is low, and puts during burning
Go out substantial amounts of harmful gas, including hydrogen sulfide, sulfur dioxide sulfides and dust etc..Therefore, efficient, clean to coal
It is imperative to utilize, it is necessary to greatly develop coal clean technology.Overall Coal Gasification combined cycle generation technology (IGCC) is one
There is the advanced clean coal technology of rosy prospect, environmental benefit is good, generating efficiency is high feature that it has.At this techniqueflow
In, the combustion gas that gasification furnace is produced is for driving gas turbine power generation, and the Steam Actuation steam turbine that fume afterheat produces generates electricity.
Typical gasification heater outlet temperature is 877 DEG C.If combustion gas can be cleaned at this temperature, the thermal efficiency of whole IGCC system will be by
It is greatly improved.On the other hand, as power plant H2S is only second to SO2Atmosphere pollution, the health of serious harm urbanite is good for
Health, removing hydrogen sulfide also will become an importance of IGCC desulfurization.Therefore the high temperature desulfurizing of coal gas is that clean coal technology grinds
One of key technology studied carefully and develop.
Charcoal-aero gel is that one is made up of nanometer spherical particle, is usually and is aggregated in the basic conditions by phenols and aldehydes
Organic aerogel, then the carbon material obtained through solvent displacement, dry, carbonization.1989, U.S.'s Lawrence National Laboratory
Room R.W.Pekala etc. with resorcinol and formaldehyde as precursor, prepare the nanometer of three dimensional structure first by sol-gal process
Aeroge.Chinese patent (application number 200610116392.3) provides the preparation method of a kind of nitrogenous charcoal-aero gel, but
Owing to it needs to be dried at supercritical conditions, comparatively laborious in technique, also limit large-scale production.
During synthesis, after there is a problem in that wet gel is formed, obtain charcoal airsetting through being dried with carbonization
Glue.Owing to the drying stress (interfacial tension) that gel pore size is huge in nanometer scale, dry run can make gel produce receipts
Contracting, even results in subsiding of hole.Therefore, in reduction gel pore, the interfacial tension of liquid, uses the drying process of safety, is to maintain
The necessary approach of gel pore structure.Supercritical Drying Technology is common technology during aeroge produces, and can eliminate gas-liquid interface, have
Effect keeps gel pore structure.But, even if using supercritical drying process to be still difficult to avoid that the generation of gel shrinks, heated
In journey, in gel pore, the expansion of liquid can cause the expansion of gel network, can cause the cracking of gel when firing rate is too fast, de-
Water shrinks and also can aggravate because of heating, thus causes the contraction of gel.Gel is frozen into solid by freeze-drying, then allows it
In solvent distillation, thus avoid the appearance of gas-liquid interface.Water in conventional dehydrated alcohol displacement gel is as solvent.This method
Need not high tension unit, thus cost is relatively low, easy and simple to handle.
The MnO form the most stable in the reducing atmosphere of 400 DEG C～1000 DEG C of manganese oxide exists, it is to avoid in hot conditions
Under make the problem of its desulphurizing activated reduction owing to generating metal simple-substance, their desulfurization to wherein part of the metal oxide simultaneously
Dynamics research finds, desulfurization rate is arranged as follows: MnO > CaO ≈ ZnO > V2O3。
IGCC process, preferably with high running temperature, has the characteristic that the desulfurizing agent of high Mn content has at high temperature had
And Sulfur capacity can be made to increase.Xue and Vriesendrop have studied particle desulfurizing agent and bulk devulcanization agent.When Fe content increases to 16%
Time, desulfurizing agent Sulfur capacity at 850 DEG C reaches 3%～5%, and when Fe content reaches 32%, Sulfur capacity is 17%.Berns etc. have studied manganese
Fimily desulfurizing agent effect in Hot gas cleanup.These can produce the low sulfur partial pressure spherical formula of renewable manganese systems in fixed bed
There are high Sulfur capacity and certain intensity, and can regenerate in many circulates.
At present, the H of research and development2S removal methods is of a great variety, such as wet desulphurization and dry desulfurization etc., Chinese patent
(ZL9410271.1) a kind of column-shaped active carbon removing H is disclosed2The method of S；Chinese patent (application number:
200610056702.7) disclose a kind of Immesion active carbon absorption H2The method of S.Chinese patent (application number:
200810200792.1) preparation method of a kind of nitrogenous carbon aerogel desulfurizing agent under normal temperature condition is disclosed, but this desulfurization
Agent is only used under normal temperature condition desulfurization and cannot accomplish that desulfurizer regeneration recycles.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of charcoal-aero gel for high temperature desulfurizing and take off
The preparation method of sulfur agent, the described this prior art to be solved of the preparation method for the carbon aerogel desulfurizing agent of high temperature desulfurizing
In desulfurizing agent be only used for the technical problem of desulfurization under normal temperature condition, to solve method of the prior art complicated simultaneously, become
This height, the technical problem that safety is the highest.
The invention provides the preparation method of a kind of carbon aerogel desulfurizing agent for high temperature desulfurizing, comprise the steps:
(1) being added in deionized water with formaldehyde by Resorcino, be subsequently adding base catalyst, described base catalyst is carbon
Acid sodium, at room temperature controlling rotating speed is that 100-450r/min stirs 2-4h, obtains the hydrosol；
Then the hydrosol of gained is put into and hermetic container is placed at 25-30 DEG C 24-36h, transfer at 45-55 DEG C the most again
Putting 24-36h, temperature controlled water baths is 65～90 DEG C and carries out sol gel reaction 48h～120h afterwards, obtains composite aquogel；
Above-mentioned Resorcino, formaldehyde, ionized water, the consumption of sodium carbonate, calculate, i.e. Resorcino: formaldehyde: ion in molar ratio
Water: sodium carbonate is 1:2:35-140:10-500；
(2), after carrying out the composite aquogel organic solvent of step (1) gained replacing 24-72h, put in freezer dryer
Under the conditions of-60～-30 DEG C, freezing 24-36h, is warming up to the 10-30 DEG C of dry 24-36h that bleeds afterwards, obtains dry organic airsetting
Glue；
Described organic solvent is any one in the tert-butyl alcohol, dehydrated alcohol or acetone；
(3) organic aerogel being dried of step (2) gained is placed in tube furnace, under nitrogen or argon, in temperature
High temperature carbonization cracking reaction 5～7h under conditions of being 800～1000 DEG C, prepares charcoal-aero gel；
(4) charcoal-aero gel of gained in step (3) is immersed in temperature be 20-35 DEG C, concentration be the manganese nitrate water of 0.5mol/L
In solution, then controlling pressure is 0.8-1.1 standard atmosphere pressure, and supersound process 2～5h, the most again by charcoal-aero gel control
Temperature is 80～150 DEG C and carries out drying 1～24h, the most under nitrogen or argon, at the bar that temperature is 800～1000 DEG C
High temperature carbonization cracking reaction 5～7h under part, obtain the carbon aerogel desulfurizing agent for high temperature desulfurizing.
Present invention also offers the carbon aerogel desulfurizing agent for high temperature desulfurizing that above-mentioned preparation method obtains.
The present invention utilizes sol-gel process, with formaldehyde and resorcinol as raw material, with natrium carbonicum calcinatum as base catalysis
Agent, water-bath generation sol gel reaction in deionized water solvent, obtain composite aquogel, solvent through organic solvent replace, close
Envelope formula lyophilization, final high temperature carbonization obtains charcoal-aero gel, after being impregnated through manganese nitrate successively by charcoal-aero gel, drying, calcine
Obtain the carbon aerogel desulfurizing agent for high temperature desulfurizing.
The carbon aerogel desulfurizing agent for high temperature desulfurizing of the present invention has bigger working sulfur capacity and saturated Sulfur capacity, can answer
H in integrated gasification combined cycle for power generation system2The high temperature removal process of S, and its to have preparation condition gentle, production sets
Standby conventional, it is suitable for the features such as large-scale production.
Due to the fact that have employed the cancellated charcoal-aero gel of 3-D makees carrier, compares more traditional Al2O3And SiO2Carry
The desulfurizing agent of body synthesis, the present invention has bigger serface and huge pore volume, remains to after the active component loading same quality
Keep good dispersibility, make Sulfur capacity be greatly improved.Compare Al2O3Carrier, charcoal-aero gel will not occur anti-with active component
Should, thus have influence on desulfurized effect.
The present invention compares with prior art, and its technological progress is significant.The charcoal airsetting for high temperature desulfurizing of the present invention
The advantages such as it is high that rubber desulfurizing agent has specific surface area, and porosity is high, Heat stability is good, thus overcome hot conditions desulfurizing agent machinery
Poor performance, the shortcoming of high temperature easy-sintering, make active component Load Balanced, and renewable use.And being used for of the present invention is high
The preparation method of carbon aerogel desulfurizing agent of temperature desulfurization has that preparation condition is controlled, preparation cost is low, safe preparation process environmental protection
Etc. advantage.
Accompanying drawing explanation
Fig. 1 is that the carbon aerogel desulfurizing agent for high temperature desulfurizing of embodiment 1 gained is worn for the desulfurizing agent of 650 DEG C of gained
Curve chart thoroughly；
Fig. 2 is that the carbon aerogel desulfurizing agent for high temperature desulfurizing of embodiment 2 gained penetrates song for the desulfurizing agent of 750 DEG C of gained
Line chart；
Fig. 3 is that the carbon aerogel desulfurizing agent for high temperature desulfurizing of embodiment 3 gained penetrates song for the desulfurizing agent of 850 DEG C of gained
Line chart.
Detailed description of the invention
Below by specific embodiment and combine accompanying drawing the present invention is expanded on further, but it is not limiting as the present invention.
Embodiment 1
The preparation method of a kind of carbon aerogel desulfurizing agent for high temperature desulfurizing, comprises the steps:
(1), Resorcino is added in deionized water with formaldehyde, be subsequently adding sodium carbonate base catalyst, the most at room temperature
Controlling rotating speed is that 300r/min stirs 2h, the hydrosol obtained；
Then the hydrosol of gained is put into and hermetic container is placed at 30 DEG C 24h, at 50 DEG C, place 24h the most again, it
Rear temperature controlled water baths is 80 DEG C and carries out sol gel reaction 48～120h, obtains composite aquogel；
Above-mentioned Resorcino, formaldehyde, ionized water, the consumption of sodium carbonate, calculate, i.e. Resorcino: formaldehyde: ion in molar ratio
Water: sodium carbonate is 1:2:45:100；
(2), by the composite aquogel organic solvent of step (1) gained carry out replacing after 72h, put in freezer dryer-
Under the conditions of 55 DEG C, freezing 30h, is warming up to 25 DEG C of dry 24h that bleed afterwards, obtains dry organic aerogel；
Described organic solvent is dehydrated alcohol；
(3), the organic aerogel being dried of step (2) gained is placed in tube furnace, in temperature under nitrogen or argon shield
It is 950 DEG C and carries out high temperature carbonization cracking 6h, prepare charcoal-aero gel；
(4), the charcoal-aero gel of gained in step (3) is immersed in temperature be 25 DEG C, concentration be that the manganese nitrate of 0.5mol/L is water-soluble
In liquid, then controlling pressure is 1 standard atmosphere pressure, and supersound process 2～5h, charcoal-aero gel controls temperature the most again is
120 DEG C carry out drying 24h, then carry out high-temperature calcination 6h at 950 DEG C under nitrogen or argon shield, obtain for high temperature desulfurizing
Carbon aerogel desulfurizing agent.
According to BET theoretical method (document Sing KSW, Everett DH, Haul RAW, Moscou L,
Pierotti RA, Rouquerol J, et al.Reporting phisisorption data for gas/solid
systems. Pure Appl Chem1985;57:603 19.) use Micromeritics ASAP 2020 instrument to above-mentioned
The carbon aerogel desulfurizing agent for high temperature desulfurizing of gained is measured, and its BET specific surface area is 433m2/g；
According to single-point method (document Sing KSW, Everett DH, Haul RAW, Moscou L, Pierotti RA,
Rouquerol J, et al.Reporting phisisorption data for gas/solid systems. Pure
Appl Chem1985;57:603 19.) use Micromeritics ASAP 2020 instrument to above-mentioned gained for high temperature
The carbon aerogel desulfurizing agent of desulfurization is measured, and its pore volume is 0.21cm3/g；
According to chromatography (document Preparation of ZnO/SiO2 gel composites and their
performance of H2S removal at room temperature.Journal of Hazardous Materials
215 216 (2012) 166 172) the GC9790IIH-2 type gas chromatograph of Zhejiang Fu Li Analytical Instrument Co., Ltd is used
Carrying out on-line analysis by the carbon aerogel desulfurizing agent the being used for high temperature desulfurizing temperature at ambient pressure of above-mentioned gained is 650 DEG C, H2S enters
Mouthful concentration 2000ppm, nitrogen content is to carry out desulfurization performance sign under conditions of 80%, when breakthrough concentration is 100ppm, examination
Test result and show that the working sulfur capacity of the carbon aerogel desulfurizing agent for high temperature desulfurizing is 100%.
By the carbon aerogel desulfurizing agent being used for high temperature desulfurizing of above-mentioned gained, for H2S fixed bed is tested, and step is as follows:
Weigh 0.2g desulfurizing agent and put into a diameter of 16mm highly for, in 800mm fixed bed glass tubing, being passed through under the conditions of 650 DEG C
Mixed gas (the 80% of N of 100ml/min2and 20% H2S)；
In above-mentioned steps gained desulfurizing agent performance characterization as it is shown in figure 1, as can be seen from Figure 1 this product be 650 in temperature
DEG C, air speed is 8000h-1, it is 2000ppmH for inlet concentration2S removes, when breakthrough concentration is 100ppm, and result of the test table
The working sulfur capacity of bright desulfurizing agent is 45.54%.
Embodiment 2
The preparation method of a kind of carbon aerogel desulfurizing agent for high temperature desulfurizing, comprises the steps:
(1), Resorcino is added in deionized water with formaldehyde, be subsequently adding sodium carbonate base catalyst, the most at room temperature
Controlling rotating speed is that 300r/min stirs 2h, the hydrosol obtained；
Then the hydrosol of gained is put into and hermetic container is placed at 30 DEG C 24h, at 50 DEG C, place 24h the most again, it
Rear temperature controlled water baths is 80 DEG C and carries out sol gel reaction 72h, obtains composite aquogel；
Above-mentioned Resorcino, formaldehyde, ionized water, the consumption of sodium carbonate, calculate, i.e. Resorcino: formaldehyde: ion in molar ratio
Water: sodium carbonate is 1:2:45:100；
(2), by the composite aquogel organic solvent of step (1) gained carry out replacing after 72h, put in freezer dryer-
Under the conditions of 55 DEG C, freezing 30h, is warming up to 25 DEG C of dry 24h that bleed afterwards, obtains dry organic aerogel；
Described organic solvent is dehydrated alcohol；
(3), the organic aerogel being dried of step (2) gained is placed in tube furnace, in temperature under nitrogen or argon shield
It is 950 DEG C and carries out high temperature carbonization cracking 6h, prepare charcoal-aero gel；
(4), the charcoal-aero gel of gained in step (3) is immersed in temperature be 25 DEG C, concentration be that the manganese nitrate of 0.5mol/L is water-soluble
In liquid, then controlling pressure is 1 standard atmosphere pressure, and supersound process 2～5h, charcoal-aero gel controls temperature the most again is
120 DEG C carry out drying 24h and do, then carry out high-temperature calcination 6h at 950 DEG C under nitrogen or argon shield, obtain for high temperature desulfurizing
Carbon aerogel desulfurizing agent.
The carbon aerogel desulfurizing agent for high temperature desulfurizing of above-mentioned gained, its BET specific surface area is 433m after measured2/ g,
Pore volume is 0.21cm3/ g, temperature is 750 DEG C at ambient pressure, H2S inlet concentration 2000ppm, under conditions of nitrogen content is 80%
Carrying out desulfurization performance sign, when breakthrough concentration is 100ppm, result of the test shows that the working sulfur capacity of desulfurizing agent is 100%.
By the carbon aerogel desulfurizing agent being used for high temperature desulfurizing of above-mentioned gained, for H2S fixed bed is tested, and step is as follows:
Weigh 0.2g desulfurizing agent and put into a diameter of 16mm highly for, in 800mm fixed bed glass tubing, being passed through under the conditions of 750 DEG C
Mixed gas (the 80% of N of 100ml/min2and 20% H2S)；
In above-mentioned steps gained desulfurizing agent performance characterization as in figure 2 it is shown, as can be seen from Figure 2 this product be 750 in temperature
DEG C, air speed is 8000h-1, it is 2000ppmH for inlet concentration2S removes, when breakthrough concentration is 100ppm, and result of the test table
The working sulfur capacity of bright desulfurizing agent is 45.54%.
Embodiment 3
The preparation method of a kind of carbon aerogel desulfurizing agent for high temperature desulfurizing, comprises the steps:
(1), Resorcino is added in deionized water with formaldehyde, be subsequently adding sodium carbonate base catalyst, the most at room temperature
Controlling rotating speed is that 300/min stirs 2h, the hydrosol obtained；
Then the hydrosol of gained is put into and hermetic container is placed at 30 DEG C 24h, at 50 DEG C, place 24h the most again, it
Rear temperature controlled water baths is 80 DEG C and carries out sol gel reaction 72h, obtains composite aquogel；
Above-mentioned Resorcino, formaldehyde, ionized water, the consumption of sodium carbonate, calculate, i.e. Resorcino: formaldehyde: ion in molar ratio
Water: sodium carbonate is 1:2:45:100；
(2), carry out replacing 72 by the composite aquogel organic solvent of step (1) gained after, put in freezer dryer-55
Under the conditions of DEG C, freezing 30h, is warming up to 25 DEG C of dry 24h that bleed afterwards, obtains dry organic aerogel；
Described organic solvent is dehydrated alcohol；
(3), the organic aerogel being dried of step (2) gained is placed in tube furnace, in temperature under nitrogen or argon shield
It is 950 DEG C and carries out high temperature carbonization cracking 6h, prepare charcoal-aero gel；
(4), the charcoal-aero gel of gained in step (3) is immersed in temperature be 25 DEG C, concentration be that the manganese nitrate of 0.5mol/L is water-soluble
In liquid, then controlling pressure is 1 standard atmosphere pressure, and supersound process 2～5h, charcoal-aero gel controls temperature the most again is
120 DEG C carry out drying 24h and do, then carry out high-temperature calcination 6h at 950 DEG C under nitrogen or argon shield, obtain for high temperature desulfurizing
Carbon aerogel desulfurizing agent.
The carbon aerogel desulfurizing agent for high temperature desulfurizing of above-mentioned gained, its BET specific surface area is 433m after measured2/ g,
Pore volume is 0.21cm3/ g, at normal pressure, temperature is 850 DEG C, H2S inlet concentration 2000ppm, nitrogen content is to enter under conditions of 80%
Row desulfurization performance characterizes, and when breakthrough concentration is 100ppm, result of the test shows that the working sulfur capacity of desulfurizing agent is 100%.
By the carbon aerogel desulfurizing agent being used for high temperature desulfurizing of above-mentioned gained, for H2S fixed bed is tested, and step is as follows:
Weigh 0.2g desulfurizing agent and put into a diameter of 16mm highly for, in 800mm fixed bed glass tubing, being passed through under the conditions of 850 DEG C
Mixed gas (the 80% of N of 100ml/min2and 20% H2S)；
In above-mentioned steps gained desulfurizing agent performance characterization as it is shown on figure 3, as can be seen from Figure 3 this product be 850 in temperature
DEG C, air speed is 8000h-1, it is 2000ppmH for inlet concentration2S removes, when breakthrough concentration is 100ppm, and result of the test table
The working sulfur capacity of bright desulfurizing agent is 60.72%.
In sum, a kind of carbon aerogel desulfurizing agent for high temperature desulfurizing that the present invention provides, from above-mentioned middle gained
Desulfurizing agent performance characterization figure can be seen that the desulfurizing agent that the present invention provides is suitable for high temperature desulfurizing, when curing temperature reaches 850 DEG C,
The working sulfur capacity of desulfurizing agent reaches to be 60.72% to the maximum.
The above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, on the premise of without departing from the technology of the present invention principle, it is also possible to make some improvement and modification, these improve and become
Type also should be regarded as protection scope of the present invention.
Claims (2)
1. the preparation method for the carbon aerogel desulfurizing agent of high temperature desulfurizing, it is characterised in that comprise the steps:
(1) being added in deionized water with formaldehyde by Resorcino, be subsequently adding base catalyst, described base catalyst is carbon
Acid sodium, at room temperature controlling rotating speed is that 100-450r/min stirs 2-4h, obtains the hydrosol；
Then the hydrosol of gained is put into and hermetic container is placed at 25-30 DEG C 24-36h, transfer at 45-55 DEG C the most again
Putting 24-36h, afterwards water-bath, control temperature is 65～90 DEG C and carries out sol gel reaction 48h～120h, obtains compound water congealing
Glue；
Above-mentioned Resorcino, formaldehyde, ionized water, the consumption of sodium carbonate, calculate, i.e. Resorcino: formaldehyde: ion in molar ratio
Water: sodium carbonate is 1:2:35-140:10-500；
(2), after carrying out the composite aquogel organic solvent of step (1) gained replacing 24-72h, put in freezer dryer
Under the conditions of-60～-30 DEG C, freezing 24-36h, is warming up to the 10-30 DEG C of dry 24-36h that bleeds afterwards, obtains dry organic airsetting
Glue；
Described organic solvent is any one in the tert-butyl alcohol, dehydrated alcohol or acetone；
(3) organic aerogel being dried of step (2) gained is placed in tube furnace, under nitrogen or argon, in temperature
High temperature carbonization cracking reaction 5～7h under conditions of being 800～1000 DEG C, prepares charcoal-aero gel；
(4) charcoal-aero gel of gained in step (3) is immersed in temperature be 20-35 DEG C, concentration be the manganese nitrate water of 0.5mol/L
In solution, then controlling pressure is 0.8-1.1 standard atmosphere pressure, and supersound process 2～5h, the most again by charcoal-aero gel control
Temperature is 80～150 DEG C and carries out drying 1～24h, the most under nitrogen or argon, at the bar that temperature is 800～1000 DEG C
High temperature carbonization cracking reaction 5～7h under part, obtain the carbon aerogel desulfurizing agent for high temperature desulfurizing.
2. the carbon aerogel desulfurizing agent for high temperature desulfurizing that the preparation method described in claim 1 obtains.
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Cited By (2)
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|---|---|---|---|---|
| CN108285135A (en) * | 2018-04-03 | 2018-07-17 | 上海电力学院 | A kind of preparation method of desulfurizing agent for high-temp gas carrier charcoal-aero gel |
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| CN108285135A (en) * | 2018-04-03 | 2018-07-17 | 上海电力学院 | A kind of preparation method of desulfurizing agent for high-temp gas carrier charcoal-aero gel |
| CN114471443A (en) * | 2021-12-28 | 2022-05-13 | 武汉大学(肇庆)资源与环境技术研究院 | Manganese oxide @ nitrogen-doped block carbon aerogel material and preparation and application thereof |
| CN114471443B (en) * | 2021-12-28 | 2023-09-29 | 武汉大学(肇庆)资源与环境技术研究院 | Manganese oxide@nitrogen doped block carbon aerogel material and preparation and application thereof |
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