CN107694535A - A kind of modified magnesia fume desulfurizing agent and preparation method thereof - Google Patents
A kind of modified magnesia fume desulfurizing agent and preparation method thereof Download PDFInfo
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- CN107694535A CN107694535A CN201711033168.2A CN201711033168A CN107694535A CN 107694535 A CN107694535 A CN 107694535A CN 201711033168 A CN201711033168 A CN 201711033168A CN 107694535 A CN107694535 A CN 107694535A
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- desulfurizing agent
- magnesia
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- modified magnesia
- powder
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular 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
- B01D53/02—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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- 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
- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/302—Sulfur oxides
Abstract
The invention discloses a kind of modified magnesia fume desulfurizing agent and preparation method thereof, by carboxymethyl chitosan, high polymer material, lauryl sodium sulfate, magnesia, tetraethyl orthosilicate, the raw materials such as ferroferric oxide powder are made, inventive desulfurization agent is coated using two kinds of organic liquors to modified magnesia, desulfurizing agent surface tension can be reduced, effectively increase gas-liquid specific surface area, improve mass transfer rate, and increase the dispersiveness of desulfurizing agent, more efficiently it can be contacted with sulfur dioxide, increase adsorption strength, improve desulfurized effect, production cost is low simultaneously, desulfuration efficiency is high, the stability of a system is strong, it can be widely used in desulfuration field.
Description
Technical field
The present invention relates to field of environment engineering technology, more particularly to a kind of modified magnesia fume desulfurizing agent and its preparation side
Method.
Background technology
Coal is in China's production of energy and consumption structure, and in occupation of leading position, its yield accounts for national energy production
The overwhelming majority, but with the continuous developing of Coal Energy Source so that the corresponding industry output large quantity of exhaust gas using coal as the energy,
These waste gas discharge in the environment, cause the pollution of environment, in the waste gas that fire coal pollutes, are occupied with the content of sulphur composition
More, this requires manufacturing enterprise to take effective sulfur method to control the pollution level of waste gas.
In numerous flue gas desulfurization techniques, a kind of de- higher as relatively ripe, desulfuration efficiency of wet process of FGD
Sulphur technology has obtained widest application.But it there is also initial cost is big, operating cost is high and the easy fouling of equipment etc.
Deficiency, and it is difficult to long-period stable operation, and accessory substance does not almost have purposes.In consideration of it, original desulphurization plant is not being entered
On the premise of row transformation and upgrade, the desulfuration efficiency of equipment is improved using desulfurizing agent, is had important practical significance.
China's magnesium ore resources enrich, about 3.1 × 10,600,000,000 tons of magnesite gross reserves, wherein about 85% concentrates on Liaoning southeast
Area.Magnesia is by system of the magnesium hydroxide extracted in magnesite stone ore, brucite mineral or seawater through high-temperature calcination, the product of sintering
Claim, its main component is MgO.Research shows that magnesia is non-isometric system periclase, and its lattice has spot defect and dislocation,
With higher surface energy, it is easy to carry out physical-chemical reaction, activity is good.MgO is in decolorizing printing and dyeing waste water processing, acid waste water
The fields such as processing, heavy metal removing, removing phosphate, deamination and flue gas desulfurization have obtained extensive research and application, wherein aoxidizing
Magnesium, with the waste gas counter current contacting containing sulfur dioxide, can generate magnesium sulfite so as to control exhaust emission in flue gas desulfurization course
Discharge.
Although magnesia material is cheap and easy to get, using it, directly as sorbing material, adsorption site is limited using then having,
And desorption easily occurs for the extension after adsorbing over time so as to influence using effect.Manganese dioxide easily with the oxygen-containing functional group such as alkyl
It is combined, adsorption site is more.But manganese dioxide particle is tiny, it is difficult to separates, limits its use range.Therefore by magnesia with
Manganese dioxide carries out mixed load and by modified technique, so as to obtain composite to greatly improve performance, turns into one
The feasible process choice of kind.
The content of the invention
The defects of the object of the invention is exactly to make up prior art, there is provided a kind of modified magnesia fume desulfurizing agent and its system
Preparation Method.
The present invention is achieved by the following technical solutions：
A kind of modified magnesia fume desulfurizing agent, is prepared by the following method：
（1）By carboxymethyl chitosan, high polymer material and water in mass ratio（12-15）：（5-6）：（7-10）It is heated to after mixing
65-75 DEG C, stir organic mother liquor A is standby；
（2）The dodecyl that mass concentration is 0.2-0.5% is added in the sodium hydrate aqueous solution for being 15-20% to mass fraction
Sodium sulphate, it is standby to be uniformly mixing to obtain organic mother liquor B；
（3）Magnesia is sent into high temperature furnace, 60-90 minutes are calcined at 500-550 DEG C, is taken out after cooling, crushed 30-40 mesh
Sieve, places into clear water and boils 30-40 minutes, filters off floating ash content and impurity in water removal after being cooled to room temperature, then be placed in dry
10-12 hours are dried in dry case, dried powder is pressed into solid-to-liquid ratio 1：It is 2.7-3.0% that 25-30g/mL, which is added to mass fraction,
Liquor potassic permanganate in, after impregnating 7-8 hours filtering take out and be sent into high temperature furnace, be warming up to 450-480 DEG C, be calcined 2-3
Hour, it is standby to obtain pre- modified magnesia powder；
（4）Pre- modified magnesia powder and tetraethyl orthosilicate are pressed into solid-to-liquid ratio 1：Stir 5-6 hours after 2-3 mixing, then divided with ultrasound
Mixed system gross mass 3-3.5% γ-chloropropyl triethoxysilane is added after dissipating, continues to be washed with clear water after stirring 5-6 hours
Wash clean, freeze-drying, by gained powder and ferroferric oxide powder 4-5 in mass ratio:Added again by 1-1.5g/L after 1 mixing
Into 20% ferric chloride solution, 20-40 minutes are shaken after ultrasonic disperse under 150-180 revs/min, clear water is rinsed well after filtering,
It is freeze-dried that must to be modified magnesia powder standby；
（5）By organic mother liquor A and organic mother liquor B 3-4 by volume：Stirred 10-15 minutes after 1 mixing, then add step thereto
The rapid modified magnesia powder of 4 gained, filters after standing 15-30 minutes, collects the magnesia powder for having coated organic liquor, produced after drying
Fume desulfurizing agent of the present invention.
High polymer material is any one in polyvinyl alcohol, polyacrylamide, polyethylene glycol oxide in the step 1.
After being impregnated in the step 3 with liquor potassic permanganate with clear water rinse it is no longer muddy to flushing water and with ultra-pure water pH
Be worth it is identical after, be placed in 60-65 DEG C of drying box dry 8-12 hours, be re-fed into high temperature furnace and carry out calcination process.
The condition of ultrasonic disperse is followed successively by ultrasonic 100-120 minutes and 35- under 25-28kHz twice in the step 4
Ultrasonic 40-60 minutes under 36kHz.
Modified magnesia powder addition is the 3-5% of mixed liquor quality in the step 5.
It is an advantage of the invention that：
The present invention is coated using two kinds of organic liquors to magnesia, wherein organic mother liquor A can reduce desulfurizing agent surface tension, is had
Effect increase gas-liquid specific surface area, improves mass transfer rate, organic mother liquor B can increase the dispersiveness of desulfurizing agent, can be more effective
Contacted with sulfur dioxide, improve desulfurized effect, the fired processing of magnesia, which is stripped of substantial amounts of absorption water and constitution water, increase, to be had
Specific surface area is imitated, while by the dip loading manganese dioxide of potassium permanganate, with reference to the two advantage, lifting composite absorption is strong
Degree, on this condition to strengthen the adsorption effect to sulfur dioxide, and ferroferric oxide magnetic powder is added into composite, and led to
Crossing the cladding of silica makes to be modified magnesia integrally firm combination, can not only increase material granule collision efficiency and frequency, by force
Change the removal to sulfureous in flue gas and other pollutants, while the recovery after materials'use can be carried out using externally-applied magnetic field, make
With convenient and efficient, inventive desulfurization agent production cost is low, and desulfuration efficiency is high, and the stability of a system is strong, can be in fields such as desulfurization
Widely use.
Embodiment
A kind of modified magnesia fume desulfurizing agent, is prepared by the following method：
（1）By carboxymethyl chitosan, polyvinyl alcohol and water in mass ratio 13：5：65 DEG C are heated to after 8 mixing, stirring to have
Machine mother liquor A is standby；
（2）The lauryl sodium sulfate that mass concentration is 0.2% is added in the sodium hydrate aqueous solution for being 15% to mass fraction,
It is standby to be uniformly mixing to obtain organic mother liquor B；
（3）Magnesia is sent into high temperature furnace, is calcined 60 minutes at 500 DEG C, is taken out after cooling, crushed 30 mesh sieves, place into
Boiled in clear water 30 minutes, filter off floating ash content and impurity in water removal after being cooled to room temperature, then be placed in drying box and dry 10
Hour, dried powder is pressed into solid-to-liquid ratio 1：25g/mL is added in the liquor potassic permanganate that mass fraction is 2.7%, dipping 7
Filtered after hour taking-up with clear water rinse to flushing water it is no longer muddy and identical with ultra-pure water pH value after, be placed in 60 DEG C of drying boxes
Dry 8 hours and be sent into high temperature furnace, be warming up to 450 DEG C, be calcined 2 hours, it is standby to obtain pre- modified magnesia powder；
（4）Pre- modified magnesia powder and tetraethyl orthosilicate are pressed into solid-to-liquid ratio 1：Stirred 5 hours after 2 mixing, then the ultrasound under 26kHz
γ-chloropropyl triethoxysilane of mixed system gross mass 3% is added after scattered 110 minutes, is used after continuing stirring 5 hours clear
Water washing is clean, freeze-drying, by gained powder and ferroferric oxide powder in mass ratio 4:It is added to again by 1g/L after 1 mixing
In 20% ferric chloride solution, ultrasonic disperse shakes 20 minutes after 60 minutes under 150 revs/min under 36kHz, and clear water rushes after filtering
Wash clean, is freeze-dried that must to be modified magnesia powder standby；
（5）By organic mother liquor A and organic mother liquor B by volume 3：Stirred 10 minutes after 1 mixing, then add mixed liquor matter thereto
Modified magnesia powder, is filtered after standing 15 minutes obtained by the step 4 of amount 3%, is collected the magnesia powder for having coated organic liquor, is dried
After produce fume desulfurizing agent of the present invention.
Claims (5)
1. a kind of modified magnesia fume desulfurizing agent, it is characterised in that be prepared by the following method：
（1）By carboxymethyl chitosan, high polymer material and water in mass ratio（12-15）：（5-6）：（7-10）It is heated to after mixing
65-75 DEG C, stir organic mother liquor A is standby；
（2）The dodecyl that mass concentration is 0.2-0.5% is added in the sodium hydrate aqueous solution for being 15-20% to mass fraction
Sodium sulphate, it is standby to be uniformly mixing to obtain organic mother liquor B；
（3）Magnesia is sent into high temperature furnace, 60-90 minutes are calcined at 500-550 DEG C, is taken out after cooling, crushed 30-40 mesh
Sieve, places into clear water and boils 30-40 minutes, filters off floating ash content and impurity in water removal after being cooled to room temperature, then be placed in dry
10-12 hours are dried in dry case, dried powder is pressed into solid-to-liquid ratio 1：It is 2.7-3.0% that 25-30g/mL, which is added to mass fraction,
Liquor potassic permanganate in, after impregnating 7-8 hours filtering take out and be sent into high temperature furnace, be warming up to 450-480 DEG C, be calcined 2-3
Hour, it is standby to obtain pre- modified magnesia powder；
（4）Pre- modified magnesia powder and tetraethyl orthosilicate are pressed into solid-to-liquid ratio 1：Stir 5-6 hours after 2-3 mixing, then divided with ultrasound
Mixed system gross mass 3-3.5% γ-chloropropyl triethoxysilane is added after dissipating, continues to be washed with clear water after stirring 5-6 hours
Wash clean, freeze-drying, by gained powder and ferroferric oxide powder 4-5 in mass ratio:Added again by 1-1.5g/L after 1 mixing
Into 20% ferric chloride solution, 20-40 minutes are shaken after ultrasonic disperse under 150-180 revs/min, clear water is rinsed well after filtering,
It is freeze-dried that must to be modified magnesia powder standby；
（5）By organic mother liquor A and organic mother liquor B 3-4 by volume：Stirred 10-15 minutes after 1 mixing, then add step thereto
The rapid modified magnesia powder of 4 gained, filters after standing 15-30 minutes, collects the magnesia powder for having coated organic liquor, produced after drying
Fume desulfurizing agent of the present invention.
2. the preparation method of modified magnesia fume desulfurizing agent according to claim 1, it is characterised in that in the step 1
High polymer material is any one in polyvinyl alcohol, polyacrylamide, polyethylene glycol oxide.
3. the preparation method of modified magnesia fume desulfurizing agent according to claim 1, it is characterised in that in the step 3
After being impregnated with liquor potassic permanganate with clear water rinse to flushing water it is no longer muddy and identical with ultra-pure water pH value after, be placed in 60-65
8-12 hours are dried in DEG C drying box, is re-fed into high temperature furnace and carries out calcination process.
4. the preparation method of modified magnesia fume desulfurizing agent according to claim 1, it is characterised in that in the step 4
The condition of ultrasonic disperse is followed successively by under 25-28kHz ultrasonic 40-60 minutes under ultrasonic 100-120 minutes and 35-36kHz twice.
5. the preparation method of modified magnesia fume desulfurizing agent according to claim 1, it is characterised in that in the step 5
Modified magnesia powder addition is the 3-5% of mixed liquor quality.
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| CN201711033168.2A CN107694535A (en) | 2017-10-30 | 2017-10-30 | A kind of modified magnesia fume desulfurizing agent and preparation method thereof |
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| CN201711033168.2A CN107694535A (en) | 2017-10-30 | 2017-10-30 | A kind of modified magnesia fume desulfurizing agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111603906A (en) * | 2020-05-18 | 2020-09-01 | 武汉理工大学 | Carbon dioxide magnesium-based adsorbent and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1390629A (en) * | 2002-07-16 | 2003-01-15 | 苏贤 | Desulfurizing agent for smoke and its preparing prcess |
| US20110143229A1 (en) * | 2006-08-24 | 2011-06-16 | Chellappa Anand S | Liquid phase desulfurization of fuels at mild operating conditions |
| CN102836636A (en) * | 2012-09-11 | 2012-12-26 | 北京世能中晶能源科技有限公司 | Desulfurization denitration composition, preparation method and application thereof |
| CN103736389A (en) * | 2013-12-12 | 2014-04-23 | 芜湖中路实业有限责任公司 | Flue gas denitration desulfurizer and preparation method thereof |
-
2017
- 2017-10-30 CN CN201711033168.2A patent/CN107694535A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1390629A (en) * | 2002-07-16 | 2003-01-15 | 苏贤 | Desulfurizing agent for smoke and its preparing prcess |
| US20110143229A1 (en) * | 2006-08-24 | 2011-06-16 | Chellappa Anand S | Liquid phase desulfurization of fuels at mild operating conditions |
| CN102836636A (en) * | 2012-09-11 | 2012-12-26 | 北京世能中晶能源科技有限公司 | Desulfurization denitration composition, preparation method and application thereof |
| CN103736389A (en) * | 2013-12-12 | 2014-04-23 | 芜湖中路实业有限责任公司 | Flue gas denitration desulfurizer and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111603906A (en) * | 2020-05-18 | 2020-09-01 | 武汉理工大学 | Carbon dioxide magnesium-based adsorbent and preparation method thereof |
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Application publication date: 20180216 |