CN107308946A - It is a kind of for shale ashes desulfurizing agent of flue gas desulfurization and preparation method thereof - Google Patents
It is a kind of for shale ashes desulfurizing agent of flue gas desulfurization and preparation method thereof Download PDFInfo
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- CN107308946A CN107308946A CN201710234400.2A CN201710234400A CN107308946A CN 107308946 A CN107308946 A CN 107308946A CN 201710234400 A CN201710234400 A CN 201710234400A CN 107308946 A CN107308946 A CN 107308946A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01D53/86—Catalytic processes
- B01D53/8603—Removing sulfur compounds
- B01D53/8609—Sulfur oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The invention discloses a kind of for shale ashes desulfurizing agent of flue gas desulfurization and preparation method thereof, desulfurizing agent is with KMnO4The shale ashes of processing are carrier, and Fe and Ce using 1 11wt% are prepared from as active component through high-temperature roasting.Its preparation method is：First shale ashes are crushed, sieves and chooses the shale lime-ash of the mesh of particle diameter 20 40；KMnO through 0.4mol/L4Solution impregnates to obtain shale ashes carrier；Shale ashes carrier is placed in 800 DEG C of high-temperature roastings, and the shale ashes carrier after roasting, which is placed in dipping in the ferric nitrate of certain concentration and cerous nitrate mixed solution, adheres to active component；Afterwards in N2Lower 800 DEG C of high-temperature roastings are protected to produce.Activity component impregnation process is 1 11wt% using 50kHz, 100W ultrasonication 0.5 2h, Fe and Ce mass fraction.The shale ashes desulfurizing agent that the present invention is implemented, cost is low, and time of break-through is up to 195min, and sulfur capacity realizes reusing for resource up to 159mg/g desulfurizing agents, is adapted in the popularization and application of flue gas desulfurization technique field.
Description
Technical field
The present invention relates to a kind of for shale ashes desulfurizing agent of flue gas desulfurization and preparation method thereof, belong to flue gas desulfurization technique
Field.
Background technology
Currently, continuing to develop with China's industry, energy-output ratio is huge, and energy resource supply is with fossils such as coal, oil
, will be using coal as main Energy Mix based on fuel, it is contemplated that following a very long time.But, the burning production of fossil fuel
Raw substantial amounts of SO2, NO and NO2Deng pollutant, harm can be brought to the mankind's production and living while pollution environment, therefore, flue gas takes off
Extensive concern of the sulphur technology by all circles.At present, flue gas desulfurization technique can be divided into two kinds of wet method and dry method, and wet desulphurization is mainly sharp
With alkaline matter such as lime stone and SO2Reaction generation calcium sulfate or calcium sulfite carry out SO2Removing, this method has reaction speed
The advantages of rate is fast, desulfuration efficiency is high, but there are high investment cost, seriously corroded and secondary pollution problems；Dry desulfurization skill
Art is mainly using the physics or chemisorbed of desulfurizing agent by SO2Removing, desulfurizing agent can carry out regeneration cycle using and have a by-product
Thing sulfuric acid, dry desulfurization has the advantages that operating cost is low, equipment corrosion is disposable by people's compared with product after light and desulfurization
Extensive concern.
Dry-desulphurizer has molecular sieve, metal oxide (such as iron-based, zinc-base, manganese base metal oxide), activated carbon etc..
As desulfurizing agent, molecular sieve is easily regenerated, and SO can be removed simultaneously2、H2S and organic sulfur compound；But molecular sieve Sulfur capacity is low, quick to steam
Sense, the presence of vapor can significantly reduce the desulphurizing activated of molecular sieve.Zinc oxide and iron oxide are industrially conventional metal oxygens
Compound desulfurizing agent, zinc oxide desulfurization temperature is general at 200-450 DEG C, with the advantage that desulfuration efficiency is high, Sulfur capacity is big, but can not be again
It is raw；By contrast, iron oxide is ambient temperature desulfuration agent, and desulfurization condition is gentle, easily regeneration, but its Sulfur capacity is not high；Activated carbon desulphurization agent
Also SO can be removed simultaneously2、H2S and organic sulfur compound, but still suffer from the application limitation that desulfuration efficiency is low, Sulfur capacity is low.
Shale ashes are the products after oil shale retorting, belong to the raw material of the similar volcanic ash containing a small amount of carbon residue, mainly into
It is divided into SiO2、Al2O3、Fe2O3, CaO, MgO etc., wherein SiO2、Al2O3Content it is higher, it is given up usually as industrial waste
Abandon, on the one hand occupied cultivated land area, and on the other hand surrounding environment is polluted.Research shows that shale ashes contain substantial amounts of acid
Property, alkalescence and amphoteric oxide, internal pore structure is flourishing, can be de- for preparing with good absorption and catalytic performance
Sulphur agent.The pattern of " treatment of wastes with processes of wastes against one another " is realized in the preparation of shale ashes desulfurizing agent, not only reduces cost, saves raw material, and desulfurization energy
Power is strong, the effective way that can be comprehensively utilized as oil shale.Current document, which yet there are no, prepares desulfurizing agent by carrier of shale ashes simultaneously
Report for flue gas desulfurization field.
The content of the invention
In order to which the raw material for solving existing desulfurizing agent presence is single, preparing the problems such as cost is high, Sulfur capacity is relatively low, there is provided one kind
The cheap easy acquisition of raw material, the shale ashes desulfurizing agent that desulfuration efficiency is high, Sulfur capacity is big and preparation method thereof.The desulfurizing agent that the present invention is provided
Have the advantages that with low cost, desulfurization performance is good, can realize resource reutilization.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of shale ashes desulfurizing agent for flue gas desulfurization, with KMnO4The shale ashes of processing are carrier, with 1-11wt%'s
Fe and Ce is supported in shale ashes as active component, active component using infusion process, and loading process uses ultrasonication.
Described shale ashes are the lime-ash after oil shale retorting, KMnO4The shale ashes of processing refer to shale ashes using leaching
Stain method is through KMnO4Handle 12h, KMnO4Solution concentration is 0.4mol/L.
Described active component loading process uses 50kHz, 100W ultrasonication, and processing time is 0.5-2h.
Present invention also offers a kind of preparation method of shale ashes desulfurizing agent, comprise the following steps：
Step one, the shale ashes for choosing certain mass crush, sieved, and choose shale ashes (SA) conduct of particle diameter 20-40 mesh
Desulfurization agent carrier, after being cleaned with deionized water, dries 12h at 110 DEG C；
Step 2, by the KMnO of shale ashes 0.4mol/L described in step one4Solution impregnates 12h, 70 DEG C of heating water bath, leaching
Stain process need to continue to stir, and form suspension；
Step 3, suspension described in step 2 is first filtered, then is cleaned several times with deionized water, until the solution after cleaning
In neutrality, 12h is then dried at 110 DEG C；
Step 4, by shale ashes described in step 3 under the conditions of 800 DEG C high-temperature roasting 2h, natural cooling, the page after cooling
Rock ash, which is marked, is；
Step 5, according to Fe and Ce load capacity, ferric nitrate and cerous nitrate quality required for calculating prepare certain concentration
Ferric nitrate and cerous nitrate solution, and the two is mixed to form mixed solution；
Step 6, NSA described in step 4 is placed in the ferric nitrate described in step 5 and cerous nitrate mixed solution, Fe matter
Amount fraction is 1-11wt%, and Ce mass fraction is 1-11wt%, and dipping process handles 0.5-2h using ultrasonic oscillation, is formed
NSA mixed solutions；
Step 7, NSA mixed solutions described in step 6 are positioned in 70 DEG C of water-baths and heated, and are stirred continuously until liquid
It is evaporated, dries 12h at 110 DEG C afterwards；
Step 8, by dried NSA described in step 7 in 800 DEG C, N2The lower high-temperature roasting 4h of protection, roasting process needs N2
Protection is produced.
The shale ashes desulfurizing agent that the present invention is provided is constituted in flue gas：O2Volume fraction 5%, SO2Entrance concentration 2000ppm,
Vapor volume fraction 10%, N2It is used as Balance Air, gas flow 400mL/min, quality of activated carbon 2g, bed reaction temperature
Under conditions of 120 DEG C, the sulfur capacity of desulfurizing agent may be up to 159mg/g desulfurizing agents, and the time of break-through of desulfurization is up to 195min, desulfurization
Agent desulfuration efficiency is high, and sulfur capacity is big, and desulfurizing agent is with low cost, and resource recycling can be achieved.
Brief description of the drawings
Fig. 1 is A classes desulfurizing agent SO provided in an embodiment of the present invention2The breakthrough curve figure of removing.
Fig. 2 is B classes desulfurizing agent SO provided in an embodiment of the present invention2The breakthrough curve figure of removing.
Fig. 3 is C classes desulfurizing agent SO provided in an embodiment of the present invention2The breakthrough curve figure of removing.
Fig. 4 is D classes desulfurizing agent SO provided in an embodiment of the present invention2The breakthrough curve figure of removing.
Fig. 5 is E classes desulfurizing agent SO provided in an embodiment of the present invention2The breakthrough curve figure of removing.
Fig. 6 evaluates the system diagram of Desulfurizer for the present invention.
In figure：1 gas cylinder (SO2, O2, N2)；2 pressure-reducing valves；3 needle valves；4 mass flowmenters；5 check valves；6 pressure gauges；7 gas
Body mixing chamber；8 steam generators；9 wet flow indicators；10 flue gas analyzers；11 cooling de-watering devices；12 temperature sensors；13 is anti-
Answer tower；14 vent gas treatments bottle.
Embodiment
The present invention can adjust active component Fe and Ce load capacity and the time of microwave treatment as needed, so as to be made
The shale ashes desulfurizing agent of different performance.
The desulfurization performance for the desulfurizing agent that the present invention is provided is evaluated using Fig. 6 systems provided.Simulated flue gas is from steel cylinder 1
Outflow is finally mixed through pressure-reducing valve 2, mass flowmenter 4 and check valve 5 in gas mixer chamber 7, is produced afterwards with steam generator 8
Vapor mixing through wet flow indicator 9 determine flow and enter reaction tower and activated carbon and react.The gas of reaction tower entrance and exit
Body composition is determined by flue gas analyzer 10, it is believed that SO2The time that exit concentration is 100ppm is time of break-through, works as exit concentration
When reaching the 95% of entrance concentration, it is believed that absorption reaches saturation.According to import and export SO2Change in concentration can draw SO2Penetrate song
Line, sulfur capacity is calculated by breakthrough curve.
Embodiment 1
The shale ashes of 2g particle diameter 20-40 mesh are weighed, are cleaned with deionized water five to eight times, its surface impurity are removed, afterwards
110 DEG C of dry 12h in drying box.Dried shale ashes are added to 0.4mol/L KMnO4In solution, KMnO4Solution is placed in
70 DEG C of heating 12h in water-bath, heating process persistently stirs to form KMnO4The suspension mixed with shale ashes.Suspension is filtered
And cleaned with deionized water, until eluate is in neutrality, 110 DEG C of dry 12h in drying box, are placed in Muffle furnace afterwards
800 DEG C of roasting 2h, produce shale ashes carrier.Load capacity according to Fe and Ce calculates the quality of ferric nitrate and cerous nitrate and prepares spy
Determine the iron nitrate solution and cerous nitrate solution of concentration, Fe and Ce mass fraction are respectively 1wt% and 2wt%, by what is prepared
Ferric nitrate and cerous nitrate solution mixing, and shale ashes carrier is added thereto dipping, dipping process uses 50kHz, and 100W's is super
Sound wave aid in treatment, ultrasonic treatment time is 60min.Then the solution after ultrasonication is placed in 70 DEG C of water-baths and heated
Until liquid is evaporated, then 110 DEG C of dry 12h in drying box are placed in, most after N2800 DEG C of roastings in Muffle furnace under protective condition
4h, is made desulfurizing agent A1.Desulfurizing agent A1For flue gas desulfurization experiment, it is in flue gas composition：O2Volume fraction 5%, SO2Entrance is dense
Spend 2000ppm, vapor volume fraction 10%, N2It is used as Balance Air, gas flow 400mL/min, quality of activated carbon 2g, bed
Under conditions of 120 DEG C of reaction temperature, the desulfurization performance of desulfurizing agent is evaluated.The breakthrough curve of desulfurizing agent is shown in Fig. 1, C0/ C tables
Show that reaction tower imports and exports SO2The ratio between concentration, desulfurizing agent A1Sulfur capacity be 72.28mg/g desulfurizing agents, time of break-through be 81min (tables
1)。
Embodiment 2-4
Be the same as Example 1, difference is that Ce load capacity is different, and Ce load capacity is 5wt%-11wt% (being shown in Table 1),
Each embodiment is made desulfurizing agent and is labeled as A2-A4.The breakthrough curve of desulfurizing agent is shown in Fig. 1, the sulfur capacity and time of break-through of desulfurizing agent
It is shown in Table 1.
The Fe and Ce of desulfurizing agent load capacity, sulfur capacity and time of break-through is made in the embodiment 1-4 of table 1.
| Embodiment | Desulfurizing agent | Fe-Ce load capacity | Sulfur capacity (mg/g desulfurizing agents) | Break through (min) |
| 1 | A1 | 1wt%-2wt% | 72.28 | 81 |
| 2 | A2 | 1wt%-5wt% | 92.87 | 108 |
| 3 | A3 | 1wt%-8wt% | 112.70 | 134 |
| 4 | A4 | 1wt%-11wt% | 82.95 | 95 |
Embodiment 5-8
Be the same as Example 1, difference is that Fe load capacity is 4wt%, and Ce load capacity (is shown in Table for 2wt%-11wt%
2), each embodiment is made desulfurizing agent and is labeled as B1-B4, and the breakthrough curve of desulfurizing agent is shown in Fig. 2, the sulfur capacity of desulfurizing agent and when penetrating
Between be shown in Table 2.
The Fe and Ce of desulfurizing agent load capacity, sulfur capacity and time of break-through is made in the embodiment 5-8 of table 2.
| Embodiment | Desulfurizing agent | Fe-Ce load capacity | Sulfur capacity (mg/g desulfurizing agents) | Break through (min) |
| 5 | B1 | 4wt%-2wt% | 102.78 | 121 |
| 6 | B2 | 4wt%-5wt% | 127.95 | 154 |
| 7 | B3 | 4wt%-8wt% | 146.25 | 178 |
| 8 | B4 | 4wt%-11wt% | 115.75 | 138 |
Embodiment 9-12
Be the same as Example 1, difference is that Fe load capacity is 7wt%, and Ce load capacity is 2wt%-11wt% (tables
3), each embodiment is made desulfurizing agent and is labeled as C1-C4, and the breakthrough curve of desulfurizing agent is shown in Fig. 3, the sulfur capacity of desulfurizing agent and when penetrating
Between be shown in Table 3.
The Fe and Ce of desulfurizing agent load capacity, sulfur capacity and time of break-through is made in the embodiment 9-12 of table 3.
| Embodiment | Desulfurizing agent | Fe-Ce load capacity | Sulfur capacity (mg/g desulfurizing agents) | Break through (min) |
| 9 | C1 | 7wt%-2wt% | 90.58 | 105 |
| 10 | C2 | 7wt%-5wt% | 136.34 | 165 |
| 11 | C3 | 7wt%-8wt% | 108.12 | 128 |
| 12 | C4 | 7wt%-11wt% | 82.95 | 95 |
Embodiment 13-16
Be the same as Example 1, difference is that Fe load capacity is 10wt%, and Ce load capacity is 2wt%-11wt%.
The Fe and Ce of desulfurizing agent load capacity, sulfur capacity and time of break-through is made in the embodiment 13-16 of table 4.
| Embodiment | Desulfurizing agent | Fe-Ce load capacity | Sulfur capacity (mg/g desulfurizing agents) | Break through (min) |
| 13 | D1 | 10wt%-2wt% | 75.33 | 85 |
| 14 | D2 | 10wt%-5wt% | 82.19 | 94 |
| 15 | D3 | 10wt%-8wt% | 127.19 | 153 |
| 16 | D4 | 10wt%-11wt% | 91.34 | 106 |
Embodiment 17-20
Be the same as Example 7, difference is that ultrasonic treatment time is different (being shown in Table 5), and desulfurizing agent mark is made in each embodiment
E1-E4 is designated as, the sulfur capacity and time of break-through of desulfurizing agent are shown in Table 5.
Ultrasonic treatment time, sulfur capacity and the time of break-through of desulfurizing agent is made in the embodiment 17-20 of table 5.
Claims (5)
1. a kind of shale ashes desulfurizing agent for flue gas desulfurization, it is characterised in that KMnO4The shale ashes of processing are carrier, Fe and Ce
As active component, active component is supported in shale ashes using infusion process, and loading process uses 50kHz, 100W ultrasonic wave
Processing, processing time is 0.5-2h；Wherein, Fe and Ce is the 1-11wt% of carrier.
2. shale ashes desulfurizing agent according to claim 1, it is characterised in that described KMnO4The shale ashes of processing refer to by
Shale ashes are using infusion process through KMnO4Handle 12h, KMnO4Solution concentration is 0.4mol/L.
3. shale ashes desulfurizing agent according to claim 1 or 2, it is characterised in that described shale ashes are oil shale retorting
Lime-ash afterwards.
4. a kind of preparation method of shale ashes desulfurizing agent for flue gas desulfurization described in claim 1 or 2 or 3, it is characterised in that
Comprise the following steps：
(1) shale ashes are chosen to crush, sieve, it is clear with deionized water using the shale ashes SA of particle diameter 20-40 mesh as desulfurizing agent raw material
After washing, 12h is dried at 110 DEG C；
(2) by step (1) shale ashes 0.4mol/L KMnO4Solution impregnates 12h, and 70 DEG C of heating water bath, dipping process is needed
Lasting stirring, forms suspension；
(3) step (2) described suspension is first filtered, then cleaned several times with deionized water, until the solution after cleaning is in neutrality,
12h is then dried at 110 DEG C；
(4) by step (3) described shale ashes high-temperature roasting 2h under the conditions of 800 DEG C, natural cooling, the shale ashes mark after cooling
For NSA；
(5) according to Fe and Ce load capacity, ferric nitrate and cerous nitrate quality required for calculating prepare the ferric nitrate of certain concentration
And cerous nitrate solution, and the two is mixed to form mixed solution；
(6) step (4) described NSA is placed in the ferric nitrate and cerous nitrate mixed solution described in step (5), Fe mass fraction
For 1-11wt%, Ce mass fraction is 1-11wt%, and dipping process handles 0.5-2h using ultrasonic oscillation, forms NSA and mixes
Close solution；
(7) step (6) the NSA mixed solutions are positioned in 70 DEG C of water-baths and heated, and be stirred continuously until that liquid is evaporated, it
12h is dried at 110 DEG C afterwards；
(8) by step (7) the dried NSA in 800 DEG C, N2The lower high-temperature roasting 4h of protection.
5. a kind of shale ashes desulfurizing agent for flue gas desulfurization is applied in flue gas desulfurization, it is characterised in that described flue gas, its
Constitute and be：O2Volume fraction 5%, SO2Entrance concentration 2000ppm, vapor volume fraction 10%, N2It is used as Balance Air, gas stream
Measure under conditions of 400mL/min, quality of activated carbon 2g, 120 DEG C of bed reaction temperature, the sulfur capacity of desulfurizing agent may be up to 159mg/
G desulfurizing agents, the time of break-through of desulfurization is up to 195min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110115921A (en) * | 2019-05-27 | 2019-08-13 | 沈阳三聚凯特催化剂有限公司 | A kind of Fe-series desulfurizing agent and preparation method thereof |
| CN111044681A (en) * | 2019-12-20 | 2020-04-21 | 中海油天津化工研究设计院有限公司 | Normal-pressure evaluation device and method for liquid desulfurizer |
| CN111189970A (en) * | 2018-11-14 | 2020-05-22 | 中国石油化工股份有限公司 | Method for detecting absorption and elimination performance of hydrogen sulfide |
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Cited By (3)
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|---|---|---|---|---|
| CN111189970A (en) * | 2018-11-14 | 2020-05-22 | 中国石油化工股份有限公司 | Method for detecting absorption and elimination performance of hydrogen sulfide |
| CN110115921A (en) * | 2019-05-27 | 2019-08-13 | 沈阳三聚凯特催化剂有限公司 | A kind of Fe-series desulfurizing agent and preparation method thereof |
| CN111044681A (en) * | 2019-12-20 | 2020-04-21 | 中海油天津化工研究设计院有限公司 | Normal-pressure evaluation device and method for liquid desulfurizer |
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