CN107262021A - The method for preparing halogen modified flying dust adsorbent - Google Patents
The method for preparing halogen modified flying dust adsorbent Download PDFInfo
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- CN107262021A CN107262021A CN201710569714.8A CN201710569714A CN107262021A CN 107262021 A CN107262021 A CN 107262021A CN 201710569714 A CN201710569714 A CN 201710569714A CN 107262021 A CN107262021 A CN 107262021A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/024—Compounds of Zn, Cd, Hg
- B01J20/0244—Compounds of Zn
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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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
- B01J20/046—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 containing halogens, e.g. halides
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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
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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
- B01D2258/0291—Flue gases from waste incineration plants
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Abstract
The present invention relates to coal-fired field, a kind of method for preparing halogen modified flying dust adsorbent is disclosed, including：Under aqueous conditions, first raw material flying dust is contacted with alkaline matter；Then products therefrom after contact is washed and dried to obtain the first intermediate；First intermediate and halogen source are subjected to immersive contact；Wherein, the specific surface area of the raw material flying dust is 0.5~2.5m2/ g, and average grain diameter is 80~200 mesh.The adsorbent obtained by the method for the present invention has excellent removal efficiency to the heavy metal Hg in coal-burning power plant's emission, and has the advantages that production cost is low.
Description
Technical field
The present invention relates to coal-fired field, and in particular to a kind of method for preparing halogen modified flying dust adsorbent.
Background technology
In recent years, because the substantial amounts of application of coal causes the control of pollution that caused by coal burning thing to turn into countries in the world focus of attention.
The metallic element mercury contained in coal, is discharged into air together with flue gas in combustion, and when can be long in an atmosphere
Between stop, and then polluted source seriously endangers health.
Coal-burning power plant is one of heavy metal Hg pollution primary discharge source, for the discharge and control of mercury, has caused the country
The concern of outer each side scholar, and conduct extensive research.A kind of way for realizing mercury control more universal at this stage
Footpath carries out Collaborative Control only with the pollutant catabolic gene such as existing desulphurization and denitration and dedusting device.
Collaborative Control technology is not to be researched and developed specifically designed for mercury pollution, and mercury pollution removal effect is difficult to ensure that stabilization.Specially
In the technology that door is removed for mercury pollution, it is to spray into solid phase before dust arrester to inhale to be best able at present close to industrial applications
Attached dose, then captured by dust arrester.
Absorbent charcoal material is to test a more class adsorbent at this stage, and it compares the capture rate to mercury in flue gas
Height, but its production cost is of a relatively high.Therefore need the sorbent material of exploitation New high-efficient low-cost badly, realize the coal-fired cigarette of removing
Heavy metal Hg pollution in gas.
The content of the invention
The invention aims to overcome prior art exist demercuration adsorbent adsorption efficiency it is not high the problem of, carry
For a kind of new method for preparing halogen modified flying dust adsorbent.
To achieve these goals, one aspect of the present invention provides a kind of method for preparing halogen modified flying dust adsorbent, bag
Include：Under aqueous conditions, first raw material flying dust is contacted with alkaline matter；Then products therefrom after contact is washed
And dry to obtain the first intermediate；First intermediate and halogen source are subjected to immersive contact；Wherein, the raw material flying dust
Specific surface area is 0.5~2.5m2/ g, and average grain diameter is 80~200 mesh.
The present inventor has found under study for action, uses specific surface area for 0.5~2.5m2/ g and average grain diameter be 80~
The raw material flying dust of 200 mesh first carries out alkali process, is then contacted with halogen source, and thus obtained adsorbent is discharged to coal-burning power plant
Heavy metal Hg in thing has excellent removal efficiency, and has the advantages that cost is low, and the technical side of the present invention is completed accordingly
Case.
Embodiment
The end points and any value of disclosed scope are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For number range, between the endpoint value of each scope, respectively
It can be combined with each other between the endpoint value of individual scope and single point value, and individually between point value and obtain one or more
New number range, these number ranges should be considered as specific open herein.
As it was previously stated, the invention provides a kind of method for preparing halogen modified flying dust adsorbent, including：In aqueous solution bar
Under part, first raw material flying dust is contacted with alkaline matter；Then products therefrom after contact is washed and dried to obtain
First intermediate；First intermediate and halogen source are subjected to immersive contact；Wherein, the specific surface area of the raw material flying dust is
0.5~2.5m2/ g, and average grain diameter is 80~200 mesh.
The specific surface area of the raw material flying dust is tested by specific surface area analysis instrument.
The aqueous conditions of the present invention refer to the system containing water, can be suspension, suspension or as clear as crystal body
System.
Dry for example can be with the condition for obtaining the drying in the first intermediate：Temperature is 70~200 DEG C, and the time is 4
~48h.
Under preferable case, the specific surface area of the raw material flying dust is 0.8~2.0m2/ g, and average grain diameter is 100~150
Mesh.
According to the first preferred embodiment, the step of raw material flying dust is contacted with alkaline matter includes：
1) raw material flying dust at a first temperature of 25~45 DEG C is first contacted into 18~24h with alkaline matter；
2) by step 1) obtained mixture contacts 6 at the second temperature than low 5~20 DEG C of first temperature~
18h。
The adsorbent obtained using the first foregoing preferred embodiment of the present invention is to coal-burning power plant's emission
In heavy metal Hg there is substantially more excellent removal efficiency.
It is further preferred that the second temperature is lower than first temperature 5~10 DEG C.
Under preferable case, the alkaline matter is sodium hydroxide and/or potassium hydroxide.
Preferably, the consumption of the alkaline matter cause the concentration of the alkaline matter in the aqueous conditions for 0.05~
5 weight %.
Under preferable case, the halogen source is at least one of halide salt selected from calcium, iron and zinc.
The halide salt of the present invention can be for example any one in chlorate, Bromide and iodized salt or many
Kind.
Under preferable case, the halogen source of the invention is calcium chloride and/or calcium bromide.
Under preferable case, the condition for controlling first intermediate to carry out immersive contact with halogen source causes by the side of the present invention
The load capacity of halogen source in the adsorbent that method is obtained is 0.5~50 weight %.Those skilled in the art can for example control solution
Concentration control the load capacity of the halogen source.
According to second of preferred embodiment, the step of first intermediate and halogen source are subjected to immersive contact
Including：
1) first intermediate and halogen source are stood into 2~8h at 10~30 DEG C；
2) by step 1) gained mixture stir 4~48h at 10~30 DEG C, and the rotating speed of the stirring be 100~
500rpm。
Preferably, the consumption of the halogen source to carry out first intermediate and halogen source in the system of immersive contact
The concentration of halogen source is 0.1~20 weight %.
Preferably, method of the invention further comprises：First intermediate and halogen source are subjected to institute after immersive contact
The product obtained dries 4~24h at 70~200 DEG C.
Under preferable case, the condition that products therefrom after contact is washed includes：The pH value for being washed to products therefrom is 7
~8；It is highly preferred that it is neutrality to be washed to products therefrom.
Under preferable case, the raw material flying dust is obtained flying dust after burning in circulating fluid bed boiler.In order that obtaining by following
The flying dust obtained after the burning of circulation fluidized bed boiler meets the requirement in technical scheme, can use and be sieved flying dust
Divide to obtain raw material flying dust of the average grain diameter as 80~200 mesh.
The composition of the raw material flying dust of the present invention for example can be：CaO content is 10.2~11.2 weight %, SiO2Contain
Measure as 50.3~54.7 weight %, Al2O3Content is 21.0~21.9 weight %, Fe2O3Content is 4.2~4.9 weight %, K2O
Content is 3.5~4.2 weight %, and content of MgO is that 0.6~0.8 weight %, MnO content is 0.04~0.08 weight %, Na2O contains
Measure as 0.7~0.95 weight % and other inevitable impurity.
The adsorbent that the method for the present invention is obtained has high absorption demercuration efficiency, and can realize that flying ash in electric power plant is secondary
Utilize.
Below will the present invention will be described in detail by preparation example, test case.
In following preparation example and test case, in case of no particular description, the various raw materials used are all from commercially available.
Preparation example 1
(1) under aqueous conditions, first by raw material flying dust, (average specific surface area is 1.2m2/ g, average grain diameter is 95 micro-
Rice) with sodium hydroxide (consumption causes the concentration of the sodium hydroxide in the aqueous conditions to be 3.5 weight %) 25 DEG C the
24h is contacted at a temperature of one；
(2) gained mixture is contacted into 10h at the second temperature than low 5 DEG C of first temperature；
(3) products therefrom progress after contact is washed into neutrality and dries 8 hours at 150 DEG C to obtain in the middle of first
Body；
(4) calcium chloride water (0~20 weight %) of first intermediate and various concentrations is stood at 20 DEG C
5h；
(5) mixture obtained by step (4) is stirred into 24h at 25 DEG C, and the rotating speed of the stirring is 400rpm；
(6) step (5) products therefrom is dried 10 hours at 150 DEG C, obtains finished product.
Respectively according to CaCl2Load capacity is 0 weight % (unsupported, for contrasting), 10 weight %, 20 weights on flying dust
Measure % and 40 weight % and prepare sample of sorbent.Unsupported flying dust and load capacity are respectively 10 weight %, 20 weight % and 40
Weight % sample is respectively labeled as FYCA0, FYCA1, FYCA2 and FYCA4.The inorganic composition content of the gained sample such as institute of table 1
Show.
Table 1
Test case 1
Coal-fired flue-gas is prepared using drop tube furnace, 30B methods sample and use Lumex RA915+Atomic absorption spectrometry
The mercury content for the sample that preparation example 1 is obtained, as a result as shown in table 2, experiment show the modification flying dust that the method for the present invention is obtained
Adsorbent has very high adsorption capacity.
Table 2
| Sample | Mercury adsorption capacity (ng/g) |
| FYCA0 | 36571 |
| FYCA1 | 523055 |
| FYCA2 | 647811 |
| FYCA4 | 605871 |
Test case 2
Hg is coordinated using the continuous mercury analyzer of PSA companies0Occurring source, carries out the sample of sorbent that preparation example 1 is obtained
The continuous adsorption penetration experiment of mercury.Specifically：
Fixed bed reactors temperature is set as 120 DEG C of constant temperature, every time filling sample of sorbent 1g.Fixed bed entrance Hg0It is dense
Spend for 40g/m2。
From experimental result surface：It is worst to the adsorption capacity of mercury without modified FYCA0 samples, do not inhale substantially
It is attached.FYCA1 samples basically reach adsorption saturation after starting absorption phase adsorption efficiency can reach 38%, 40h.FYCA2 and
FYCA4 properties of sample close to and it is more excellent, initial adsorption efficiency close to 60% and time of break-through in 80h or so.
Preparation example 2
(1) under aqueous conditions, first by raw material flying dust, (average specific surface area is 1.3m2/ g, average grain diameter is 82 micro-
Rice) with sodium hydroxide (consumption causes the concentration of the sodium hydroxide in the aqueous conditions to be 2.5 weight %) 35 DEG C the
22h is contacted at a temperature of one；
(2) gained mixture is contacted into 14h at the second temperature than low 7 DEG C of first temperature；
(3) products therefrom progress after contact is washed into neutrality and dries 6 hours at 180 DEG C to obtain in the middle of first
Body；
(4) by solution of calcium bromide in water (0 weight %, 5 weight %, the 10 weight % of first intermediate and various concentrations
With 20 weight %) stand 4h at 25 DEG C；
(5) mixture obtained by step (4) is stirred into 30h at 20 DEG C, and the rotating speed of the stirring is 300rpm；
(6) step (5) products therefrom is dried 8 hours at 180 DEG C, obtains finished product.
5 weight %, 10 weight % and 20 weight % of unsupported flying dust and use maceration extract (solution of calcium bromide in water)
To sample be respectively labeled as FYCB0, FYCB1, FYCB2 and FYCB3.The inorganic composition content of gained sample is as shown in table 3.
Table 3
Test case 3
Coal-fired flue-gas is prepared using drop tube furnace, 30B methods sample and use Lumex RA915+Atomic absorption spectrometry
The mercury content for the sample that preparation example 2 is obtained, as a result as shown in table 4, experiment show the modification flying dust that the method for the present invention is obtained
Adsorbent has very high adsorption capacity.
Table 4
| Sample | Mercury adsorption capacity (ng/g) |
| FYCB0 | 38309 |
| FYCB1 | 1023055 |
| FYCB2 | 1247811 |
| FYCB3 | 1805871 |
Test case 4
Hg is coordinated using the continuous mercury analyzer of PSA companies0Occurring source, carries out the sample of sorbent that preparation example 2 is obtained
The continuous adsorption penetration experiment of mercury.Specifically：
Fixed bed reactors temperature is set as 120 DEG C of constant temperature, every time filling sample of sorbent 1g.Fixed bed entrance Hg0It is dense
Spend for 40g/m2。
From experimental result surface：It is worst to the adsorption capacity of mercury without modified FYCB0 samples, do not inhale substantially
It is attached.FYCB1 samples basically reach adsorption saturation after starting absorption phase adsorption efficiency can reach 45%, 35h.FYCB2 and
FYCB3 properties of sample close to and it is more excellent, initial adsorption efficiency close to 75% and time of break-through in 65h or so.
Preparation example 3
This preparation example is carried out using the method similar to preparation example 2, except that：The step of this preparation example (1) and step
Suddenly (2) are respectively：
(1), first will (consumption causes described with the identical raw material flying dust of preparation example 2 and sodium hydroxide under aqueous conditions
The concentration of sodium hydroxide in aqueous conditions is 2.5 weight %) contact 22h at a first temperature of 35 DEG C；
(2) gained mixture is contacted into 14h at the second temperature than low 2 DEG C of first temperature；
Remaining is identical with preparation example 2, and the concentration of the solution of calcium bromide in water in this preparation example is 5 weight %.
Using the mercury adsorption capacity for the sample of sorbent that the acquisition of this preparation example is tested with the identical method of testing of test case 3,
As a result it is：801268ng/g.
Preparation example 4
This preparation example is carried out using the method similar to preparation example 3, except that：
The step of this preparation example (1) and step (2) are respectively：
(1), first will (consumption causes described with the identical raw material flying dust of preparation example 2 and sodium hydroxide under aqueous conditions
The concentration of sodium hydroxide in aqueous conditions is 2.5 weight %) contact 22h at a first temperature of 35 DEG C；
(2) gained mixture is continued under 25 DEG C of second temperature to contact 14h；
Remaining is identical with preparation example 3, and the concentration of the solution of calcium bromide in water in this preparation example is 5 weight %.
Using the mercury adsorption capacity for the sample of sorbent that the acquisition of this preparation example is tested with the identical method of testing of test case 3,
As a result it is：755641ng/g.
Contrast preparation example 1
This contrast preparation example is carried out using the method similar to preparation example 1, except that：
The average specific surface area of raw material flying dust in this contrast preparation example is 1.5m2/ g, average grain diameter is 51 microns.
Remaining is identical with preparation example 1.
Adsorbed and held using the mercury for the sample of sorbent that the acquisition of this contrast preparation example is tested with the identical method of testing of test case 1
Amount, as a result for：482530ng/g.
The adsorbent that the method for the present invention is obtained it can be seen from the above results has high absorption demercuration efficiency, and
Preparation method is simple, with low cost.
The preferred embodiment of the present invention described in detail above, still, the present invention is not limited thereto.In the skill of the present invention
In art concept, technical scheme can be carried out a variety of simple variants, including each technical characteristic with it is any its
Its suitable method is combined, and these simple variants and combination should equally be considered as content disclosed in this invention, belong to
Protection scope of the present invention.
Claims (10)
1. a kind of method for preparing halogen modified flying dust adsorbent, including：Under aqueous conditions, first by raw material flying dust and alkalescence
Material is contacted；Then products therefrom after contact is washed and dried to obtain the first intermediate；By in described first
Mesosome carries out immersive contact with halogen source；Wherein, the specific surface area of the raw material flying dust is 0.5~2.5m2/ g, and average grain diameter is
80~200 mesh.
2. the method according to claim 1, wherein, the step of raw material flying dust is contacted with alkaline matter includes：
1) raw material flying dust at a first temperature of 25~45 DEG C is first contacted into 18~24h with alkaline matter；
2) by step 1) obtained mixture contacts 6~18h at the second temperature than low 5~20 DEG C of first temperature.
3. method according to claim 2, wherein, the second temperature is lower than first temperature 5~10 DEG C.
4. the method according to any one in claim 1-3, wherein, the alkaline matter is sodium hydroxide and/or hydrogen
Potassium oxide；Preferably,
The consumption of the alkaline matter causes the concentration of the alkaline matter in the aqueous conditions to be 0.05~5 weight %.
5. the method according to any one in claim 1-3, wherein, the halogen source is the halogenation selected from calcium, iron and zinc
At least one of salt；Preferably,
The halogen source is calcium chloride and/or calcium bromide.
6. the method according to any one in claim 1-3, wherein, first intermediate is impregnated with halogen source
The step of contact, includes：
1) first intermediate and halogen source are stood into 2~8h at 10~30 DEG C；
2) by step 1) gained mixture stirs 4~48h at 10~30 DEG C, and the rotating speed of the stirring is 100~500rpm.
7. according to the method described in claim 1, wherein, the consumption of the halogen source to enter first intermediate with halogen source
The concentration of halogen source in the system of row immersive contact is 0.1~20 weight %；Preferably 1~10 weight %.
8. according to the method described in claim 1, wherein, this method further comprises：First intermediate is entered with halogen source
The product of gained dries 4~24h at 70~200 DEG C after row immersive contact.
9. according to the method described in claim 1, wherein, the condition that products therefrom after contact is washed includes：It is washed to
The pH value of products therefrom is 7~8.
10. according to the method described in claim 1, wherein, the raw material flying dust is to obtain after burning in circulating fluid bed boiler
Flying dust.
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| CN107262021B (en) | 2020-02-18 |
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