CN105833829B - A kind of modification type porous calcium carbonate adsorbent and its preparation method and application - Google Patents
A kind of modification type porous calcium carbonate adsorbent and its preparation method and application Download PDFInfo
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- CN105833829B CN105833829B CN201610243205.1A CN201610243205A CN105833829B CN 105833829 B CN105833829 B CN 105833829B CN 201610243205 A CN201610243205 A CN 201610243205A CN 105833829 B CN105833829 B CN 105833829B
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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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
- B01J20/28054—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 surface properties or porosity
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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
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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
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
Abstract
The invention discloses a kind of modification type porous calcium carbonate adsorbents for belonging to purifying coal-fired flue gas technical field and its preparation method and application.The modification type porous calcium carbonate adsorbent, using bromide as dressing agent, dipping modification is carried out to porous calcium carbonate using the porous calcium carbonate that SDS is template preparation as matrix, and grinding after drying is made, in the deep purifying that can be applied to coal-fired flue-gas.The adsorbent has larger specific surface area, can adsorb majority of gas and particulate matter, especially sour gas such as SO simultaneously2、SO3, condensable particulate matter and Hg0.Calcium carbonate after adsorption saturation can return to limestone slurry liquid preparing system, be used as new desulfurization absorbent, and adsorbed product SO3 2‑、SO4 2‑, condensable particulate matter then become calcium sulfite or calcium sulfate and enter slurries, finally enter gypsum, not will produce secondary pollution, prepare low raw-material cost, it is simple for process, easily realize industrialization.
Description
Technical field
The invention belongs to purifying coal-fired flue gas technical fields, and in particular to a kind of modification type porous calcium carbonate adsorbent and its
Preparation method and application.
Background technology
The situation is tense for current China's atmosphere pollution, and the pollutant of the energy resource structure discharge based on coal causes many regions
Haze takes place frequently and is on the rise.Now the mainstream technology of domestic purifying coal-fired flue gas be by low nitrogen burning, SCR, high-effective dust-removing and
Wet desulphurization is sequentially connected in series, and is formed flue gas multiple pollutant and is jointly controlled system.But the effect of the system is single, it can not be to flue gas
Middle condensable particulate matter (predominantly SO3) and heavy metal Hg processing, and still have SO2、NOxIt is remained with dust.Although extensive
Unit has been mounted with above-mentioned smoke gas treatment equipment, but medium and small boiler flue gas polution control facility operation is in poor shape, inorganization row
It is serious to put phenomenon, is not effectively controlled so far.
Meanwhile " most tight in history "《Fossil-fuel power plant atmospheric pollutant emission standard》Executed, all fire coals before the year two thousand twenty
Power plant must realize that minimum discharge, wherein sulfur dioxide are no more than 35mg/m3, nitrogen oxides be no more than 50mg/m3, flue dust do not surpass
Cross 5mg/m3.And it is not included in SO therein now3Discharge capacity be 40-200mg/m3, the primary pollution that will become in coal-fired flue-gas
Object.Therefore, (the predominantly SO of the condensable particulate matter in coal-fired flue-gas3) caused by gypsum rain problem and heavy metal Hg dirt
Dye etc. needs us and solves.
Invention content
The purpose of the present invention is to provide a kind of modification type porous calcium carbonate adsorbents and its preparation method and application, take
Technical solution it is as follows：
A kind of modification type porous calcium carbonate adsorbent, the porous calcium carbonate that the adsorbent is prepared using SDS as template
For matrix, using bromide as dressing agent.
The bromide is NH4Br or NaBr.
The preparation method of the modification type porous calcium carbonate adsorbent, specifically includes following steps：
(1) under magnetic agitation, PH to 6.5~11 is adjusted after calcium chloride water and SDS aqueous solutions are quickly mixed, is obtained
Emulsus mixed liquor；
(2) emulsus mixed liquor is persistently stirred, and aqueous sodium carbonate is added, stands 4-8 hours, forms white precipitate, it is right
White precipitate is centrifuged, washs to obtain porous calcium carbonate；
(3) dipping modification is carried out to porous calcium carbonate with bromide solution, the modification of white powder shape is obtained after drying and grinding
Type porous calcium carbonate adsorbent.
A concentration of 0.1-0.4mol/L of the calcium chloride water；The calcium chloride water rubs with SDS aqueous solutions
You are than being (4:1)-(1:1)；The molar ratio of the aqueous sodium carbonate and calcium chloride water is (4:1)-(1:1).
The rotating speed of step (2) described centrifugation is 2000-3000rpm, time 2-3min；The concrete mode of the washing
For：Using respectively washing three times of deionized water and absolute ethyl alcohol.
The mass fraction of bromide is 1%-5% in bromide solution described in step (3).
Dry temperature described in step (3) is 55-85 DEG C, and the time is 10-12 hours.
Application of the modification type porous calcium carbonate adsorbent in coal-fired flue-gas deep purifying.
The modification type porous calcium carbonate adsorbent can adsorb the SO in coal-fired flue-gas3、SO2With metal Hg；It is wherein right
SO3Adsorption efficiency 90% or more.
Limestone slurry liquid preparing system is returned to after the modification type porous calcium carbonate adsorbent adsorption saturation, as new
Desulfurization absorbent uses, and adsorbed product SO3 2-、SO4 2-, condensable particulate matter then becomes calcium sulfite or calcium sulfate and enters slurry
Liquid finally enters gypsum.
Modification type porous calcium carbonate adsorbent described in 1g is after absorption starts 5min, to SO3Adsorption rate 70% with
On, to Hg0Adsorption efficiency be not less than 95%.
Beneficial effects of the present invention are：
(1) specific surface area of the modification type porous calcium carbonate adsorbent is larger, and adsorption effect is notable, in coal-fired flue-gas
SO3Adsorption efficiency can reach 90% or more, and can effectively remove polar molecule (such as SO readily soluble in flue gas2) and heavy metal Hg
Equal multi-pollutants.
(2) limestone slurry liquid preparing system is can return to after the modification type porous calcium carbonate adsorbent adsorption saturation described in, is made
It is used for new desulfurization absorbent, and adsorbed product SO2-、SO3-, condensable particulate matter then become calcium sulfite or calcium sulfate into
Enter slurries, finally enters gypsum, not will produce secondary pollution.
(3) modification type porous calcium carbonate adsorbent manufacturing cost of the invention is cheap, and preparation process is simple, absorption efficiency
Height easily recycles.Without considering the problems of adsorbent reactivation, operating cost is greatly reduced, China's coal fired power plant, enlargement are suitble to
Work enterprise, metallurgy industry realize minimum discharge and the transformation of medium and small boiler flue gas polution control facility, have promotional value.
Description of the drawings
Fig. 1 is that modification type porous calcium carbonate adsorbent prepared by embodiment 1 adsorbs SO3Breakthrough curve figure.
Fig. 2 is that modification type porous calcium carbonate adsorbent prepared by embodiment 2-6 adsorbs SO3Breakthrough curve figure.
Fig. 3 is that modification type porous calcium carbonate adsorbent prepared by embodiment 7-9 adsorbs Hg0Breakthrough curve figure.
Specific implementation mode
The present invention will be further described with reference to the accompanying drawings and examples, and but the scope of the present invention is not limited thereto.
The test method of the adsorption efficiency of modification type porous calcium carbonate adsorbent is as follows：The a certain amount of adsorbent is taken to be added
Into fixed bed reactors, it is passed through a certain amount of SO3With Hg0The mixed gas of steam is reacted, and the gas of fixed bed reactors is passed through
Body is absorbed with sodium hydroxide solution and tail gas collection system is arranged.Reaction condition is：The flow velocity of mixed gas is 0.2L/
Min, reaction temperature are 65 DEG C.The concentration and mercury ion content of reactor exit sulfate radical are measured at interval of a period of time,
It is passed through SO in gas3Amount and sodium hydroxide solution in the difference of content of sulfate radical be the SO absorbed in fixed bed reactors3
Amount, thus obtains certain time SO3Absorption efficiency, can similarly obtain Hg0Absorption efficiency.
Embodiment 1
Under magnetic agitation, by the 0.15mol/L CaCl of same volume2Aqueous solution and 0.1moL/L SDS aqueous solutions are quick
PH to 9 is adjusted after mixing, obtains emulsus mixed liquor；
Emulsus mixed liquor is persistently stirred, is added and the isometric 0.2mol/L Na of mixed solution2CO3It is small to stand 6 for aqueous solution
When, form white precipitate；White precipitate is collected by centrifugation, is used in combination deionized water to be washed respectively three times with absolute ethyl alcohol, obtains porous carbon
Sour calcium；
It uses mass fraction to carry out dipping modification to porous calcium carbonate for 1% NaBr solution, dries, grind in 60 DEG C of baking ovens
The modification type porous calcium carbonate adsorbent of white powder shape is obtained after mill.
Obtained adsorbent is added in 5 parallel fixed bed reactors, the dosage of adsorbent be respectively 0.4g,
0.6g, 0.8g, 1.0g, 1.2g compare its adsorption effect under identical reaction conditions.Using adsorption efficiency and adsorbance come table
It levies adsorbent and adsorbs SO3Ability, test result indicates with breakthrough curve.The ordinate of curve is SO in the gas of exit3Concentration
(c) with inlet SO3Initial concentration (c0) between ratio (c/c0× 100%), adsorption efficiency is：(1-c/c0) × 100%,
Breakthrough curve illustrates that, by the concentration variation of absorbed component, absorption result is as shown in Figure 1.
From fig. 1, it can be seen that adsorbent of the present invention is to SO3There is significant adsorption efficiency.When the adsorbent amount from
When 0.4g increases to 1.2g, the 5min after absorption starts, fixed bed reactors exit SO3Concentration and initial SO3The ratio between concentration from
57% is reduced to 0.2%, i.e. SO3Adsorption efficiency be increased to 98.8% from 53%.
Embodiment 2
Under magnetic agitation, by the 0.15mol/L CaCl of same volume2Aqueous solution and 0.1moL/L SDS aqueous solutions are quick
PH to 9 is adjusted after mixing, obtains emulsus mixed liquor；
Emulsus mixed liquor is persistently stirred, is added and the isometric 0.2mol/L Na of mixed solution2CO3It is small to stand 8 for aqueous solution
When, form white precipitate；White precipitate is collected by centrifugation, is used in combination deionized water to be washed respectively three times with absolute ethyl alcohol, obtains porous carbon
Sour calcium；
Use mass fraction for 1% NH4Br solution carries out dipping modification to porous calcium carbonate, is dried in 60 DEG C of baking ovens,
The modification type porous calcium carbonate adsorbent of white powder shape is obtained after grinding.
The 1.0g adsorbents prepared are added in fixed bed reactors, the adsorbent adsorbs SO3Breakthrough curve such as
Shown in Fig. 2.It can be seen that the 5min after absorption starts, the adsorbent is to SO3Adsorption efficiency be 94.5%.
Embodiment 3
Under magnetic agitation, by the 0.1mol/L CaCl of same volume2Aqueous solution and 0.1moL/L SDS aqueous solutions quickly mix
PH to 9 is adjusted after conjunction, obtains emulsus mixed liquor；
Emulsus mixed liquor is persistently stirred, is added and the isometric 0.2mol/L Na of mixed solution2CO3It is small to stand 8 for aqueous solution
When, form white precipitate；White precipitate is collected by centrifugation, is used in combination deionized water to be washed respectively three times with absolute ethyl alcohol, obtains porous carbon
Sour calcium；
Use mass fraction for 1% NH4Br solution carries out dipping modification to porous calcium carbonate, is dried in 60 DEG C of baking ovens,
The modification type porous calcium carbonate adsorbent of white powder shape is obtained after grinding.
The 1.0g adsorbents prepared are added in fixed bed reactors, the adsorbent adsorbs SO3Breakthrough curve such as
Shown in Fig. 2.It can be seen that the 5min after absorption starts, the adsorbent is to SO3Adsorption efficiency be 90%.
Embodiment 4
Under magnetic agitation, by the 0.2mol/L CaCl of same volume2Aqueous solution and 0.1moL/L SDS aqueous solutions quickly mix
PH to 9 is adjusted after conjunction, obtains emulsus mixed liquor；
Emulsus mixed liquor is persistently stirred, is added and the isometric 0.2mol/L Na of mixed solution2CO3It is small to stand 8 for aqueous solution
When, form white precipitate；White precipitate is collected by centrifugation, is used in combination deionized water to be washed respectively three times with absolute ethyl alcohol, obtains porous carbon
Sour calcium；
Use mass fraction for 1% NH4Br solution carries out dipping modification to porous calcium carbonate, is dried in 60 DEG C of baking ovens,
The modification type porous calcium carbonate adsorbent of white powder shape is obtained after grinding.
The 1.0g adsorbents prepared are added in fixed bed reactors, the adsorbent adsorbs SO3Breakthrough curve such as
Shown in Fig. 2.It can be seen that the 5min after absorption starts, the adsorbent is to SO3Adsorption efficiency be 84%.
Embodiment 5
With vigorous stirring, by the 0.2mol/L CaCl of same volume2Aqueous solution and 0.05moL/L SDS aqueous solutions are fast
PH to 9 is adjusted after speed mixing, obtains emulsus mixed liquor；
Emulsus mixed liquor is persistently stirred, is added and the isometric 0.2mol/L Na of mixed solution2CO3It is small to stand 8 for aqueous solution
When, form white precipitate；White precipitate is collected by centrifugation, is used in combination deionized water to be washed respectively three times with absolute ethyl alcohol, obtains porous carbon
Sour calcium；
Use mass fraction for 1% NH4Br solution carries out dipping modification to porous calcium carbonate, is dried in 60 DEG C of baking ovens,
The modification type porous calcium carbonate adsorbent of white powder shape is obtained after grinding.
The 1.0g adsorbents prepared are added in fixed bed reactors, the adsorbent adsorbs SO3Breakthrough curve such as
Shown in Fig. 2.It can be seen that the 5min after absorption starts, the adsorbent is to SO3Adsorption efficiency be 76%.
Embodiment 6
Under magnetic agitation, by the 0.3mol/L CaCl of same volume2Aqueous solution and 0.1moL/L SDS aqueous solutions quickly mix
PH to 9 is adjusted after conjunction, obtains emulsus mixed liquor；
Emulsus mixed liquor is persistently stirred, is added and the isometric 0.2mol/L Na of mixed solution2CO3It is small to stand 8 for aqueous solution
When, form white precipitate；White precipitate is collected by centrifugation, is used in combination deionized water to be washed respectively three times with absolute ethyl alcohol, obtains porous carbon
Sour calcium；
Use mass fraction for 1% NH4Br solution carries out dipping modification to porous calcium carbonate, is dried in 60 DEG C of baking ovens,
The modification type porous calcium carbonate adsorbent of white powder shape is obtained after grinding.
The 1.0g adsorbents prepared are added in fixed bed reactors, the adsorbent adsorbs SO3Breakthrough curve such as
Shown in Fig. 2.It can be seen that the 5min after absorption starts, the adsorbent is to SO3Adsorption efficiency be 71%.
Embodiment 7
Under magnetic agitation, by the 0.15mol/L CaCl of same volume2Aqueous solution and 0.1moL/L SDS aqueous solutions are quick
PH to 9 is adjusted after mixing, obtains emulsus mixed liquor；
Emulsus mixed liquor is persistently stirred, is added and the isometric 0.2mol/L Na of mixed solution2CO3It is small to stand 4 for aqueous solution
When, form white precipitate；White precipitate is collected by centrifugation, is used in combination deionized water to be washed respectively three times with absolute ethyl alcohol, obtains porous carbon
Sour calcium；
Use mass fraction for 1% NH4Br solution carries out dipping modification to porous calcium carbonate, is dried in 60 DEG C of baking ovens,
The modification type porous calcium carbonate adsorbent of white powder shape is obtained after grinding.
The 1.0g adsorbents prepared are added in fixed bed reactors, the adsorbent adsorbs Hg0Breakthrough curve such as
Shown in Fig. 3.The ordinate of curve is Hg in the gas of exit0Concentration (c) and inlet Hg0Initial concentration (c0) between ratio
(c/c0× 100%), adsorption efficiency is：(1-c/c0) × 100%.It can be seen that the 5min after absorption starts, the adsorbent
To Hg0Adsorption efficiency be 99.3%.
Embodiment 8
Under magnetic agitation, by the 0.15mol/L CaCl of same volume2Aqueous solution and 0.1moL/L SDS aqueous solutions are quick
PH to 9 is adjusted after mixing, obtains emulsus mixed liquor；
Emulsus mixed liquor is persistently stirred, is added and the isometric 0.2mol/L Na of mixed solution2CO3It is small to stand 4 for aqueous solution
When, form white precipitate；White precipitate is collected by centrifugation, is used in combination deionized water to be washed respectively three times with absolute ethyl alcohol, obtains porous carbon
Sour calcium；
Use mass fraction for 3% NH4Br solution carries out dipping modification to porous calcium carbonate, is dried in 60 DEG C of baking ovens,
The modification type porous calcium carbonate adsorbent of white powder shape is obtained after grinding.
The 1.0g adsorbents prepared are added in fixed bed reactors, the adsorbent adsorbs Hg0Breakthrough curve such as
Shown in Fig. 3.It can be seen that the 5min after absorption starts, the adsorbent is to Hg0Adsorption efficiency be 98%.
Embodiment 9
Under magnetic agitation, by the 0.15mol/L CaCl of same volume2Aqueous solution and 0.1moL/L SDS aqueous solutions are quick
PH to 9 is adjusted after mixing, obtains emulsus mixed liquor；
Emulsus mixed liquor is persistently stirred, is added and the isometric 0.2mol/L Na of mixed solution2CO3It is small to stand 4 for aqueous solution
When, form white precipitate；White precipitate is collected by centrifugation, is used in combination deionized water to be washed respectively three times with absolute ethyl alcohol, obtains porous carbon
Sour calcium；
Use mass fraction for 5% NH4Br solution carries out dipping modification to porous calcium carbonate, is dried in 60 DEG C of baking ovens,
The modification type porous calcium carbonate adsorbent of white powder shape is obtained after grinding.
The 1.0g adsorbents prepared are added in fixed bed reactors, the adsorbent adsorbs Hg0Breakthrough curve such as
Shown in Fig. 3.It can be seen that the 5min after absorption starts, the adsorbent is to Hg0Adsorption efficiency be 95%.
Claims (9)
1. a kind of modification type porous calcium carbonate adsorbent, which is characterized in that the adsorbent prepares more using SDS as template
Hole calcium carbonate is matrix, using bromide as dressing agent；
The modification type porous calcium carbonate adsorbent is prepared with the following method：
(1) under magnetic agitation, pH to 6.5~11 is adjusted after calcium chloride water and SDS aqueous solutions are quickly mixed, obtains breast
Shape mixed liquor；
(2) emulsus mixed liquor is persistently stirred, and aqueous sodium carbonate is added, stands 4-8 hours, white precipitate is formed, to white
Precipitation is centrifuged, washs to obtain porous calcium carbonate；
(3) dipping modification carried out to porous calcium carbonate with bromide solution, it is dry after grinding obtain white powder shape modification type it is more
Hole calcium carbonate adsorbent.
2. a kind of modification type porous calcium carbonate adsorbent according to claim 1, which is characterized in that the bromide is
NH4Br or NaBr.
3. a kind of modification type porous calcium carbonate adsorbent according to claim 1, which is characterized in that the calcium chloride is water-soluble
A concentration of 0.1-0.4mol/L of liquid；The molar ratio of the calcium chloride water and SDS aqueous solutions is (4:1)-(1:1)；It is described
The molar ratio of aqueous sodium carbonate and calcium chloride water is (4:1)-(1:1).
4. a kind of modification type porous calcium carbonate adsorbent according to claim 1, which is characterized in that step (2) it is described from
The rotating speed of the heart is 2000-3000rpm, time 2-3min；The concrete mode of the washing is：Using deionized water and anhydrous second
Alcohol respectively washing three times.
5. a kind of modification type porous calcium carbonate adsorbent according to claim 1, which is characterized in that step (3) described bromine
The mass fraction of bromide is 1%-5% in salting liquid.
6. a kind of modification type porous calcium carbonate adsorbent according to claim 1, which is characterized in that described in step (3)
Dry temperature is 55-85 DEG C, and the time is 10-12 hours.
7. application of the modification type porous calcium carbonate adsorbent in coal-fired flue-gas deep purifying described in claim 1.
8. application according to claim 7, which is characterized in that the modification type porous calcium carbonate adsorbent can adsorb combustion
SO in flue-gas3、SO2With metal Hg；Wherein to SO3Adsorption efficiency 90% or more.
9. application according to claim 7, which is characterized in that after the modification type porous calcium carbonate adsorbent adsorption saturation
Limestone slurry liquid preparing system is returned, is used as new desulfurization absorbent, and adsorbed product SO3 2-、SO4 2-, condensable particle
Object then becomes calcium sulfite or calcium sulfate enters slurries, finally enters gypsum.
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| CN101985099A (en) * | 2010-11-22 | 2011-03-16 | 东南大学 | Flue gas demercuration adsorbent and preparation method thereof |
| CN103372418A (en) * | 2012-04-28 | 2013-10-30 | 东南大学 | Modified activated carbon demercuration adsorbent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101985099A (en) * | 2010-11-22 | 2011-03-16 | 东南大学 | Flue gas demercuration adsorbent and preparation method thereof |
| CN103372418A (en) * | 2012-04-28 | 2013-10-30 | 东南大学 | Modified activated carbon demercuration adsorbent and preparation method thereof |
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| Title |
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| 碳酸钙纳米结构多孔空心微球的制备及其药物缓释性能研究;李亮等;《无机材料学报》;20090131;第24卷(第1期);第166-170页 * |
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