CN106669670B - A kind of preparation method of fume desulfurizing agent - Google Patents
A kind of preparation method of fume desulfurizing agent Download PDFInfo
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- CN106669670B CN106669670B CN201510761658.9A CN201510761658A CN106669670B CN 106669670 B CN106669670 B CN 106669670B CN 201510761658 A CN201510761658 A CN 201510761658A CN 106669670 B CN106669670 B CN 106669670B
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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
- B01J23/72—Copper
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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 preparation methods of fume desulfurizing agent, including following content: 1) cupric maceration extract being divided into two parts maceration extract A and maceration extract B, first impregnate macropore precursor with maceration extract A, then impregnate macropore precursor with siliceous solution, then drying for standby；(2) by step (1) resulting material and boehmite dry glue powder, chemical enlargement agent, extrusion aid, peptizing agent kneading at plastic, extrusion, drying, then high-temperature process in an oxygen-free atmosphere roast in oxygen-containing atmosphere, obtain modified aluminium oxide supports；(3) modified aluminium oxide supports obtained with maceration extract B impregnation steps (2) through drying, roast obtained fume desulfurizing agent.The fume desulfurizing agent of this method preparation, active component is reasonably distributed in carrier channel surfaces, Sulfur capacity with higher and desulphurizing activated, has broad application prospects in Dry FGD.
Description
Technical field
The present invention relates to a kind of preparation methods of fume desulfurizing agent.
Background technique
With the continuous development of industry, demand of the mankind to the energy increasingly increases, and obtains the approach of the energy although more,
Still based on the burning of fuel.The energy in China is mainly from the burning of fossil fuel-coal, it is contemplated that, will in decades from now on
It is still the main composition of China's energy.Boiler is the capital equipment for converting the chemical energy of fuel to thermal energy, Industrial Boiler flue gas
Discharging major pollutants is flue dust and sulfur dioxide, and according to statistics, 80% and sulfur dioxide (SO2) emissions of atmospheric aerosol total emission volumn are total
The 90% of amount is all from burning of coal, and acid rain occurs to some extent in overwhelming majority area.
Currently, for flue gas SO2Existing more than 100 kinds of emission control technique, wet process and two kinds of dry method can be divided into,
The wherein lime stone in wet process (lime)-gypsum, has obtained large-scale business application, accounts for about the existing flue gas desulfurization in the world
The 85% of device.Nevertheless, that there are still one-time investments is excessively high, operating cost is expensive, water consumption is big, raw for the Wet technique
At gypsum easily cause secondary pollution, take up a large area, exhaust temperature relatively low the disadvantages of needing reheating to discharge fume after desulfurization, therefore develop
Efficient desulfurization by dry method has been a hot spot of research.
Dry desulfurizing process is mostly by the SO in adsorbent adsorbing and removing flue gas2, after inhaling sulphur saturation, desulfurizing agent is carried out again
Raw, the desulfurizing agent after regeneration is reused for desulfurization, constitutes closed cycle, and when regeneration, sulphur is mostly with high concentration SO2Form put
Out, sulphur, liquid SO can be further processed into2Or therefore sulfuric acid utilizes Sulphur ressource, in turn avoid the transfer of waste, shows
Extremely strong prospects for commercial application is shown.
CuO/Al in desulfurization by dry method2O3Flue gas desulfurization technique is of increasing concern, early in the sixties in last century, lotus
Blue SHELL company just starts porous aluminium oxide loaded copper oxide (CuO/Al2O3) desulfurizing agent research.CN101181684A is public
A kind of absorbing catalyst and preparation method thereof for flue gas desulfurization is opened, the absorbing catalyst is with γ-Al2O3For carrier, at it
Area load copper oxide and cerium oxide, wherein the amount of copper oxide is γ-Al2O3Quality 2.5-15.0%, the γ-of cerium oxide
Al2O3Quality 2.5-15.0%.The absorbing catalyst of this method preparation, since addition Ce is as co-catalyst, to CuO/ γ-
Al2O3Catalyst is modified, and increases the absorbing catalyst service life.CN101559367A discloses a kind of removing SO2With NOx's
Integrated absorbing catalyst and preparation method thereof, it is main using the γ-Al with strong adsorption capacity and catalytic activity2O3As desulfurization
Agent carrier, co-catalyst are binary composite metal salt and Zn (NO3)2, different component is prepared for by incipient impregnation method
CuO/γ-Al2O3Absorption/catalyst, the desulfurizing agent not only have good removing SO2Effect, and to NOxAlso have good
Removal effect.CN1375355A discloses a kind of SO removed in flue gas2The desulfurizing agent and its preparation process of gas, desulfurizing agent
With metal oxide (oxide of copper, zinc, iron, sodium, nickel, titanium etc.) for main component, there is the DS01 type for being attached to carrier and each
One-time formed two kinds of DS02 type of ingredient mixing.The preparation process of DS01 type is first prepared with Al2O3、ZnO、NiO、TiO2、Na2O
For the carrier of component, after metal oxide is attached on carrier；The preparation process of DS02 type is by metal oxide, activation
It is desulfurizing agent that agent, adhesive and pore creating material etc., which mix one-pass molding,.
The above technology is applied in flue gas desulfurization, achieves preferable effect, but the desulfuration efficiency of above-mentioned desulfurizing agent and
Sulfur capacity needs to improve.Due to desulphurization reaction be it is internally deep from particle surface, belong to it is interior diffusion controlling reaction,
And excessively high copper-loaded amount also easily causes blockage of the micro orifice and macropore undergauge, therefore how to make active component more reasonable on carrier
Distribution, weaken in spread influence, improve the overall utilization rate of active component, become improve the active pass of Dry FGD
Key.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of fume desulfurizing agent, the cigarette of this method preparation
Gas desulfurizer, active component are reasonably distributed in carrier channel surfaces, Sulfur capacity with higher and desulphurizing activated, anti-in flue gas desulfurization
It is had broad application prospects in answering.
The preparation method of fume desulfurizing agent of the invention, including following content:
(1) cupric maceration extract is divided into two parts maceration extract A and maceration extract B, first impregnates macropore precursor with maceration extract A, then
Macropore precursor is impregnated with siliceous solution, then drying for standby；
(2) by step (1) resulting material and boehmite dry glue powder, chemical enlargement agent, extrusion aid, peptizing agent kneading at
Plastic, extrusion, drying, then high-temperature process in an oxygen-free atmosphere roast in oxygen-containing atmosphere, obtain modified aluminium oxide supports；
(3) modified aluminium oxide supports obtained with maceration extract B impregnation steps (2) through drying, roast obtained flue gas desulfurization
Agent.
In the method for the present invention, copper content in maceration extract A described in step (1) is calculated as final desulfurizing agent weight with copper oxide
The 1wt%-10wt% of amount, preferably 2wt% ~ 5wt%.Wherein maceration extract is formulated as making in maceration extract known to those skilled in the art
Mantoquita is generally one or more of copper nitrate, copper acetate or copper chloride etc..
In the method for the present invention, siliceous solution described in step (1) is the ethanol solution containing esters of silicon acis, and wherein esters of silicon acis is selected from
One or more of methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester or butyl silicate.
In the method for the present invention, the solid-liquid mass ratio of macropore precursor described in step (1) and siliceous solution is 1:5 ~ 1:30.
In the method for the present invention, mass ratio of the silicon source in terms of silica with macropore precursor is 5:1~1 described in step (1):
1。
In the method for the present invention, macropore precursor described in step (1) is aluminium carbonate ammonium, carbon black powder, starch, cellulose or activity
One or more of carbon fiber, preferably aluminium carbonate ammonium；Wherein the mesh number of carbon black powder, starch, cellulose or activated carbon fiber is
100 ~ 300 mesh, preferably 150 ~ 250 mesh.Macropore precursor is preferably through aluminium salt and/or ammonia salt aqueous solution impregnation, dipping side
Formula can use isometric or cross volume impregnation, and dip time is 1-3 hours；The aluminium salt is aluminum nitrate, aluminum sulfate or chlorine
Change one of aluminium or a variety of, preferably aluminum nitrate, the concentration of aluminum salt solution is 1wt% ~ 30wt%, preferably 5wt% ~ 25wt%；
The ammonium salt can be the mixing of one or more of ammonium carbonate, ammonium hydrogen carbonate, ammonium oxalate, and the concentration of ammonium salt aqueous solution is 2-
10mol/L, preferably 3-7mol/L.
In the method for the present invention, drying condition described in step (1) are as follows: 20 ~ 100 DEG C of drying temperature, preferably 50 ~ 80 DEG C are done
The dry time is 1-24 hours, preferably 3 ~ 12 hours.
In the method for the present invention, the additional amount for the material that step (1) obtains in step (2) is boehmite dry glue powder weight
10%-20%.
In the method for the present invention, chemical enlargement agent described in step (2) is one of phosphoric acid, phosphate or boric acid or several
Kind, preferably phosphate, wherein phosphate is selected from one or more of ammonium phosphate, ammonium hydrogen phosphate or ammonium dihydrogen phosphate, and chemistry expands
Agent additional amount in hole is the 3%-5% of boehmite dry glue powder weight.
In the method for the present invention, extrusion aid described in step (2) is one of sesbania powder, starch or methylcellulose or several
Kind, preferably sesbania powder, extrusion aid additional amount are the 3%-5% of boehmite dry glue powder weight.
In the method for the present invention, peptizing agent described in step (2) is one of formic acid, acetic acid, citric acid or nitric acid or several
Kind mixing, additional amount is the 3%-10% of boehmite dry glue powder weight, depending on last molding effect.
In the method for the present invention, step (2) drying condition is 1-24 hours dry at 100-130 DEG C.
In the method for the present invention, oxygen-free atmosphere described in step (2) is inert atmosphere, N2, CO or CO2Etc. one of atmosphere
Or it is several, oxygen-free atmosphere high-temperature process temperature is 350 ~ 450 DEG C, and the processing time is 2 ~ 8 hours.
In the method for the present invention, oxygen-containing atmosphere described in step (2) is generally the mixture or oxygen of air, oxygen and nitrogen
One of with the mixture of inert gas, the volume fraction of oxygen in the gas phase is 20% ~ 40%.The maturing temperature is
350~800 DEG C, preferably 500~700 DEG C, calcining time are 2~8 hours, preferably 3~5 hours.
In the method for the present invention, maceration extract B described in step (3) can use volume impregnation, incipient impregnation or spray
Impregnating mode, dip time are 1-5 hours, the specific concentration of maceration extract can according to the tenor on final catalyst and
It is fixed.
In the method for the present invention, drying condition described in step (3) is 2-24 hours dry at 80-120 DEG C；The roasting
Condition is to roast 3-10 hours at 400-600 DEG C.
The method of the present invention also can according to need during the preparation process be added Na, K, Ca, Sr, Ba, La, Ce, Fe, Co, Ni,
One or more of auxiliary agents such as Zn, Cr or V, promoter addition based on the element, account for 0.5wt% ~ 5wt% of desulfurizing agent weight.
The fume desulfurizing agent of the method for the present invention preparation, in terms of desulfurizing agent weight percent, including following component: copper oxide 4%
~ 18%, preferably 6% ~ 13%, silica 1% ~ 10%, preferably 2% ~ 6%, surplus are alumina support.
The fume desulfurizing agent of the method for the present invention preparation is applied in Dry FGD, general process conditions are as follows: oxygen
Volume fraction be 2%-10%, entrance SO2Concentration is 500-2500mg/m3, 250-550 DEG C of reaction temperature, preferably 350-400 DEG C,
Reaction velocity 500-5000h-1, preferably 1000-3000h-1。
The method of the present invention successively pre-processes macropore precursor using amount of activated component maceration extract, siliceous solution, in kneading
It during preparing alumina support, is heat-treated by anaerobic, so that silicon source comes into full contact with aluminium oxide, and is converted into titanium dioxide
Silicon removes macropore precursor, while reaming, SiO further by calcination process2Remain stuck to the big of macropore precursor formation
Hole surface is played a supporting role, and the intensity of alumina support, while SiO are enhanced2Modifying function, reduce active component
Interaction with alumina carrier surface and the acidity for improving macroporous aluminium oxide surface, improve the activity of catalyst,
Additionally, due to SiO2Supporting role ensure that the intensity of aluminium oxide macropore so that alumina support be not easy to collapse then again with it is quasi-
Boehmite and other auxiliary agent kneadings；Macropore precursor is gradually aoxidized, decomposes, is escaped in roasting process simultaneously, participates in macropore
It generates, active metal component is loaded in corresponding macropore in macropore precursor, then by double-steeping active component, is increased
Active component content at desulfurizing agent macropore, improves the utilization rate of macropore in desulfurizing agent, improve desulfurizing agent activity and
Sulfur capacity, the gas that macropore precursor by modification etc. generates when thermally decomposing plays good reaming effect, and improves
The connectivity of macropore easily enters the gas molecules such as sulfur dioxide in desulfurizing agent macropore duct, weakens the interior influence spread, mentions
The overall utilization rate of high-activity component further improves Dry FGD activity, has in Dry FGD wide
Application prospect.
Specific embodiment
Below will by embodiment, invention is further explained, but it is not thereby limiting the invention.It can basis
The additional amount for needing to adjust soluble copper salt prepares the maceration extract of various concentration.
Embodiment 1
(1) the aluminium carbonate ammonium (in terms of final desulfurizing agent weight, CuO load capacity is 0.5 gram) for taking 11 grams of dipping CuO, is added
Into the ethanol solution containing ethyl orthosilicate, (wherein solid-liquid mass ratio is 1:8, and ethyl orthosilicate is with SiO2Meter and carbon black powder
Mass ratio is 2:1), it impregnation 1 hour, filters, it is 2 hours dry at 50 DEG C of solid phase, obtain modified aluminium carbonate ammonium；
(2) the modification aluminium carbonate ammonium for obtaining step (1) and boehmite dry glue powder (aluminium oxide contents on dry basis 70%)
150 grams, 5 grams of sesbania powders, 2 grams of ammonium phosphate are uniformly mixed, then kneading is added and continues to mix dissolved with the aqueous solution of 5 grams of nitric acid in right amount
Pinch, form, it is 3 hours dry in 120 DEG C, 5 then in nitrogen 400 DEG C handle 3 hours, 500 DEG C of roastings 5 are small in air atmosphere
When, modified aluminium oxide supports are made；
(3) 100 grams of modified aluminium oxide supports are weighed, is carried with 150 milliliters of 5 grams/100 milliliters copper nitrate solution dippings containing CuO
Body 2 hours, redundant solution is filtered off, 115 DEG C dry 2 hours, then roast 5 hours obtained desulfurizing agent A, the desulfurizing agent at 550 DEG C
CuO is 5wt%, and surplus is alumina support.
Embodiment 2 ~ 5
With embodiment 1, the difference is that pore creating material used in each embodiment is different, copper oxide and silica content difference,
Each embodiment desulfurizing agent number is respectively B ~ E, and pore-creating dosage, copper oxide and silica content used in each embodiment are shown in Table 1.
Comparative example 1
Material amounts prepare copper-containing alumina carrier with embodiment 1, using a step infusion process, without the use of pre-soaked portion
The macropore precursor for dividing copper and silicon, obtains desulfurizing agent F.Desulfurizing agent composition is shown in Table 1.
Comparative example 2
With embodiment 1, only no siliceous solution dipping process and anaerobic high-temperature process, obtain desulfurizing agent G.Desulfurizing agent group
At being shown in Table 1.
Embodiment 6
Above-mentioned desulfurizing agent A ~ G is applied to Dry FGD, reaction evaluating condition are as follows: the volume fraction of oxygen is 5%,
400 DEG C of reaction temperature, reaction velocity 3000h-1, entrance SO2Concentration is 1000mg/m3, evaluation result is shown in Table 2.
1 macropore precursor dosage of table and active component content.
[1] benchmark is the percentage for accounting for boehmite weight.
[2] benchmark is the percentage for accounting for desulfurizing agent weight.
[3] dipping process is to use ammonium carbonate solution (concentration 3mol/L), is impregnated 2 hours, drying for standby.
The evaluation result of each embodiment of table 2 and comparative example desulfurizing agent.
Claims (16)
1. a kind of preparation method of fume desulfurizing agent, it is characterised in that including following content: (1) cupric maceration extract being divided into two
Divide maceration extract A and maceration extract B, first impregnates macropore precursor with maceration extract A, then impregnate macropore precursor with siliceous solution, then dry
It is spare；(2) by step (1) resulting material and boehmite dry glue powder, chemical enlargement agent, extrusion aid, peptizing agent kneading at can
Plastomer, extrusion, drying, then high-temperature process in an oxygen-free atmosphere roast in oxygen-containing atmosphere, obtain modified aluminium oxide supports；(3)
The modified aluminium oxide supports obtained with maceration extract B impregnation steps (2) through drying, roast obtained fume desulfurizing agent.
2. according to the method for claim 1, it is characterised in that: the copper content in maceration extract A described in step (1), with oxygen
Change the 1wt%-10wt% that copper is calculated as final desulfurizing agent weight.
3. according to the method for claim 1, it is characterised in that: the copper content in maceration extract A described in step (1), with oxygen
Change 2wt% ~ 5wt% that copper is calculated as final desulfurizing agent weight.
4. according to the method for claim 1, it is characterised in that: siliceous solution described in step (1) is the second containing esters of silicon acis
Alcoholic solution, wherein esters of silicon acis is selected from one of methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester or butyl silicate or several
Kind.
5. according to the method for claim 1, it is characterised in that: macropore precursor described in step (1) is consolidated with siliceous solution
Liquid mass ratio is 1:5 ~ 1:30；The silicon source is 5:1~1:1 with the mass ratio of macropore precursor in terms of silica.
6. according to the method for claim 1, it is characterised in that: macropore precursor described in step (1) is aluminium carbonate ammonium, carbon black
One or more of powder, starch, cellulose or activated carbon fiber.
7. according to the method for claim 6, it is characterised in that: carbon black powder, starch, cellulose or the activated carbon fiber
Mesh number be 100 ~ 300 mesh.
8. according to the method for claim 1, it is characterised in that: the macropore precursor is water-soluble by aluminium salt and/or ammonium salt
Liquid impregnation, impregnation method use isometric or cross volume impregnation, and dip time is 1-3 hours；The aluminium salt is nitric acid
One of aluminium, aluminum sulfate or aluminium chloride are a variety of, and the concentration of aluminum salt solution is 1wt% ~ 30wt%；The ammonium salt is carbonic acid
The mixing of one or more of ammonium, ammonium hydrogen carbonate, ammonium oxalate, the concentration of ammonium salt aqueous solution are 2-10mol/L.
9. according to the method for claim 1, it is characterised in that: drying condition described in step (1) are as follows: drying temperature 20 ~
100 DEG C, drying time is 1-24 hours.
10. according to the method for claim 1, it is characterised in that: the additional amount for the material that step (1) obtains in step (2)
For the 10%-20% of boehmite dry glue powder weight.
11. according to the method for claim 1, it is characterised in that: chemical enlargement agent described in step (2) is phosphoric acid, phosphoric acid
One or more of salt or boric acid, chemical enlargement agent additional amount are the 3%-5% of boehmite dry glue powder weight；Step (2)
The extrusion aid is one or more of sesbania powder, starch or methylcellulose, and extrusion aid additional amount is boehmite
The 3%-5% of dry glue powder weight；Peptizing agent described in step (2) is that one or more of formic acid, acetic acid, citric acid or nitric acid are mixed
It closes, additional amount is the 3%-10% of boehmite dry glue powder weight.
12. according to the method for claim 1, it is characterised in that: oxygen-free atmosphere described in step (2) is inert atmosphere, nothing
Oxygen atmosphere high-temperature process temperature is 350 ~ 450 DEG C, and the processing time is 2 ~ 8 hours.
13. according to the method for claim 12, it is characterised in that: inert atmosphere described in step (2) is N2, CO or CO2Gas
One or more of atmosphere.
14. according to the method for claim 1, it is characterised in that: oxygen-containing atmosphere described in step (2) be air, oxygen with
One of mixture or oxygen and the mixture of inert gas of nitrogen, the volume fraction of oxygen in the gas phase are 20% ~ 40%；
The maturing temperature is 350~800 DEG C, and calcining time is 2~8 hours.
15. the fume desulfurizing agent prepared according to method described in claim 1 ~ 14 any claim, it is characterised in that: with de-
Sulphur agent weight percent meter, including following component: copper oxide 4% ~ 18%, silica 1% ~ 10%, surplus are alumina support.
16. it is anti-to be applied to flue gas desulfurization according to the fume desulfurizing agent of the preparation of method described in claim 1 ~ 14 any claim
Ying Zhong, process conditions are as follows: the volume fraction of oxygen is 2%-10%, entrance SO2Concentration is 500-2500mg/m3, reaction temperature 250-
550 DEG C, reaction velocity 500-5000h-1。
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| CN109603472B (en) * | 2018-11-29 | 2021-03-23 | 河北彩客化学股份有限公司 | Adsorbent and method for treating waste gas containing sulfur dioxide |
| CN111330424B (en) * | 2020-01-20 | 2020-11-27 | 北京宝聚能源科技有限公司 | Flue gas desulfurizing agent and preparation method and application thereof |
| CN113750759A (en) * | 2021-10-08 | 2021-12-07 | 成都龙飞科技有限公司 | Preparation method of combined desulfurizer, combined desulfurizer and desulfurization method |
| CN115253623A (en) * | 2022-08-22 | 2022-11-01 | 哈密市鲁江缘新材料有限公司 | Desulfurizing agent and preparation method and application thereof |
| CN117563556B (en) * | 2024-01-16 | 2024-04-02 | 北京北大先锋科技股份有限公司 | Renewable load-type desulfurizing agent and preparation method thereof |
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