CN106669354A - Mercury removal adsorbent for flue gas as well as preparation method and application thereof - Google Patents

Mercury removal adsorbent for flue gas as well as preparation method and application thereof Download PDF

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Publication number
CN106669354A
CN106669354A CN201611119518.2A CN201611119518A CN106669354A CN 106669354 A CN106669354 A CN 106669354A CN 201611119518 A CN201611119518 A CN 201611119518A CN 106669354 A CN106669354 A CN 106669354A
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CN
China
Prior art keywords
adsorbent
powder
copper chloride
demercuration
preparation
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CN201611119518.2A
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Chinese (zh)
Inventor
周子健
刘小伟
徐明厚
廖志强
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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Priority to CN201611119518.2A priority Critical patent/CN106669354A/en
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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
    • 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
    • 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
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • 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
    • 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

Abstract

The invention discloses a mercury removal adsorbent for flue gas as well as a preparation method and application thereof. The mercury removal adsorbent is prepared from 85 weight percent to 97 weight percent of Ce(1-x)ZrxO2 powder and 3 weight percent to 15 weight percent of copper chloride, wherein the grain diameter of the Ce(1-x)ZrxO2 powder is 20mum to 200mum; the copper chloride is loaded on the surface of the Ce(1-x)ZrxO2 powder. In a preparation process of the mercury removal adsorbent, calcination is not needed; the preparation method is simple and the activity of the copper chloride can be guaranteed; meanwhile, consumption of energy sources is reduced; when the mercury removal adsorbent is used for a low-chlorine or chlorine-free atmosphere, the mercury removal efficiency can still keep 80 percent or more for 10h under the condition that the air speed ratio of 380000h<-1>.

Description

A kind of demercuration adsorbent for flue gas and preparation method and application
Technical field
The invention belongs to atmospheric cleaning field, more particularly, to a kind of demercuration adsorbent for flue gas and its preparation Method and application.
Background technology
Used as the main consuming energy of China, it is main in air that the hydrargyrum of coal-burning power plant's discharge is that human activity is discharged into coal Source, the hydrargyrum discharged into the atmosphere can be enriched with human body after entering biosphere, serious harm health.Due in China's coal Content of halogen is low, and halogen is the catalysis oxidation and the key factor of absorption of hydrargyrum, therefore for coal-fired flue-gas adsorbent demercuration Mainly halogen modified mineral or synthesizing new adsorbent, for example, be modified to mineral or adsorbent using copper chloride.
But the adsorbent of prior art and catalyst choose the metal-oxides such as cerium oxide, copper oxide, cobalt oxide or Chabasie is used as carrier；And on these carrier surfaces, the active o content of chemisorbed is low, therefore the copper chloride for loading cannot Sufficiently activated, preferable demercuration effect cannot be then obtained in low chlorine or free from chloride coal-fired flue-gas.
For example, patent documentation CN105749937A discloses a kind of based on natural crystal, metal-oxide and copper chloride Catalyst.The preparation process of the catalyst is complicated, needs through multi-load；Meanwhile, when using barium oxide as load When, catalyst has stronger toxicity, easily causes secondary pollution to environment.Patent documentation CN102101007A discloses one kind Catalyst based on the modified oxidized cobalt of copper chloride.The Land use systems of catalyst prepared by the method are the catalyst of powder and take off Sulfur Gypsum Fibrosum mixes, it is difficult to separate with desulfurated plaster, therefore more difficult recovery, regeneration, and departs from the flue-gas temperature in tower less than 200 DEG C, and the optimum activity temperature range of copper chloride is 200 DEG C~250 DEG C in catalyst, its activity is not at optimum activity temperature It is interval.The modified natural crystal demercuration adsorbent of copper chloride is reported in patent documentation CN105498688A, prepared by the adsorbent During there is high-temperature burning process, easily cause the inactivation of copper chloride, so as to affect the performance of adsorbent, and calcination process Expend the substantial amounts of energy.
And though cerium zirconium based solid solution is applied to absorption (such as patent documentation of the toxic gas such as NOx CN104492414A), yet with cerium zirconium sosoloid when for flue gas demercuration, need using the chlorine unit contained in flue gas in itself Element as oxidant, its in low chlorine or without chlorine flue gas in then there is relatively low demercuration activity.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the present invention proposes a kind of demercuration adsorbent for flue gas And preparation method and application, its object is to solve demercuration adsorbent for low chlorine even the mercury removal efficiency of free from chloride flue gas Not high problem, its core technology are the Ce using high active oxygen content(1-x)ZrxO2As demercuration adsorbent it is main into Point, so as to the hydrargyrum in oxidation removal flue gas.
For achieving the above object, according to one aspect of the present invention, there is provided a kind of demercuration adsorbent for flue gas, bag Include the Ce of 85wt.%~97wt.%(1-x)ZrxO2The copper chloride of powder and 3wt.%~15wt.%, the Ce(1-x)ZrxO2Powder The particle diameter at end is 20 μm~200 μm, and the copper chloride is carried on the Ce(1-x)ZrxO2Powder surface.
Preferably, in the Ce(1-x)ZrxO2In, x is 0~0.5.
As it is further preferred that in the Ce(1-x)ZrxO2In, x is 0.3~0.4, to avoid due to CeO2Content is very few So as to affect the quantity of the Lacking oxygen of demercuration adsorbent, and then the performance of impact adsorbent, and ZrO2The very few impact of content Ce(1-x)ZrxO2Stability so that the service life of demercuration adsorbent shortens.
Preferably, the demercuration adsorbent includes the copper chloride of 6wt.%~10wt.%；To avoid the quality point of copper chloride Number is too low and produce Cu-lyt. in use, and mass fraction is too high and copper chloride occur on demercuration adsorbent surface Crystal, so as to affect the oxidation susceptibility of copper chloride, affects the activity of the demercuration adsorbent then.
Preferably, the demercuration adsorbent is cellular or tabular.
Used as it is further preferred that the demercuration adsorbent is for cellular, its length is 1000mm~1500mm, its section For rectangle, the length of side of the rectangle is 200mm~300mm, and the cellular aperture is 3mm~10mm, wall thickness be 1mm~ 2mm。
As it is further preferred that the demercuration adsorbent that obtains in step S3 is tabular, its thickness be 0.5mm~ 1mm, length are 1000mm~1500mm, and width is 500mm~650mm.
According to one aspect of the present invention, a kind of preparation method of above-mentioned demercuration adsorbent, including following step are additionally provided Suddenly：
S1. by Ce(1-x)ZrxO2Powder infusion is more than the copper chloride solution 3min of 10g/L~500g/L in concentration, makes institute State Ce(1-x)ZrxO2The area load copper oxide of powder, and the copper oxide and Ce of the load(1-x)ZrxO2The mass ratio of powder is 3:97~3:17；
S2. the Ce of copper chloride will be loaded with(1-x)ZrxO2Powder is fully dried, and obtains the demercuration adsorbent.
Preferably, copper chloride solution and Ce in step S1(1-x)ZrxO2The volume of powder is equal, the dipping when Between be 5min~10min so that the copper oxide and Ce of the load(1-x)ZrxO2The mass ratio of powder is 3:47~1:9.
Preferably, method fully dry in step S2 is：More than 24h, Ran Hou are kept first below 30 DEG C 50 DEG C~75 DEG C of temperature heating 6h~12h, it is to avoid high temperature drying causes vapor rapid evaporation, brings the chlorination of load copper The loss of amount simultaneously affects the form of demercuration adsorbent.
Preferably, the Ce(1-x)ZrxO2Powder is prepared with sol-gal process, to ensure Ce(1-x)ZrxO2The grain of powder Footpath and composition are more uniform.
Preferably, also including step S3 after step S2：By the demercuration adsorbent be compressed to it is cellular or Tabular.
Preferably, the atmosphere being fully dried in step S2 is air.
It is another aspect of this invention to provide that additionally providing a kind of application of above-mentioned demercuration adsorbent in the demercuration of flue gas.
In general, by the contemplated above technical scheme of the present invention compared with prior art, with following beneficial effect Really：
1st, the present invention is with Ce(1-x)ZrxO2Used as the main component of demercuration adsorbent, and demercuration adsorbent is loaded with high activity Copper chloride；Therefore, the demercuration adsorbent goes for the coal-fired flue-gas of any chlorinity；It is prepared by empirical tests, the present invention Even if demercuration adsorbent in for low chlorine or free from chloride atmosphere (such as N2+ 6%O2+100μg/m3The flue gas atmosphere of Hg) when, Air speed ratio is 380000h- 1Under conditions of, 10h later demercuration efficiency remains to keep more than 80%；
2nd, due to needing not move through calcining, preparation method is simple, and avoids high temperature shadow for the preparation process of demercuration adsorbent The activity of copper chloride is rung, while reducing the consumption of the energy.
Description of the drawings
Fig. 1 is the structural representation of cellular adsorbent prepared by the embodiment of the present invention 1.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention Limit the present invention.As long as additionally, technical characteristic involved in invention described below each embodiment each other it Between do not constitute conflict can just be mutually combined.
The invention provides a kind of demercuration adsorbent for flue gas and preparation method and application；Its preparation method includes Following steps：
S1. choose cerium zirconium based solid solution (the i.e. Ce that particle diameter is 20 μm~200 μm(1-x)ZrxO2) powder infusion is in copper chloride More than solution 3min, makes the Ce(1-x)ZrxO2The area load copper oxide of powder；The concentration of the copper chloride solution is 10g/L ~500g/L, concentration and the time of dipping of copper chloride solution can affect Ce(1-x)ZrxO2The load capacity of powder；The time of dipping Preferably 5min~10min, now, Ce(1-x)ZrxO2If powder impregnated in isopyknic copper chloride solution it is adsorbable about 95% copper chloride；Dip time is long or excessive concentration can cause the mass fraction of copper oxide higher, otherwise then low； Ce(1-x)ZrxThe particle diameter of O powder is preferably 50 μm~100 μm, and particle diameter is excessive, may cause the specific surface area of demercuration adsorbent compared with It is little so as to affect its absorption property, and particle diameter is too small, then can affect the cyclical stability of mercury absorbent；
S2. the Ce of copper chloride will be loaded with(1-x)ZrxO2Powder is fully dried, and obtains the demercuration adsorbent；In order to avoid One time high temperature drying causes vapor rapid evaporation, brings the loss of the chlorination copper mass of load and affects the shape of demercuration adsorbent State；More than 24h can be kept below 30 DEG C first in dry run, then in 50 DEG C~75 DEG C of temperature holding 6h~12h；It is dried Atmosphere ensures anacidity alkali-free, generally directly can be dried in air atmosphere；
S3. the demercuration adsorbent is compressed to into cellular or flat demercuration adsorbent, so as in coal-burning power plant Economizer or electrostatic precipitator after carry out using when be easy to dismounting.
The Ce in step S1.(1-x)ZrxO2In powder, x is 0~0.5；Due to CeO2Content is crossed The quantity of the Lacking oxygen of adsorbent, and then the performance of adsorbent is affected, and ZrO2Content crosses the Ce for making generation at least(1-x)ZrxO2No It is stable so that demercuration adsorbent easily fails, therefore when x is 0.3~0.4, the performance of demercuration adsorbent is optimal；And Ce(1-x) ZrxO2Powder is preferably prepared with sol-gal process, to ensure Ce(1-x)ZrxO2The particle diameter and composition of powder is more uniform.
The demercuration adsorbent that method described above is prepared, empirical tests include the Ce of 85wt.%~97wt.%(1-x)ZrxO2 The copper chloride of powder and 3wt.%~15wt.%；And when copper chloride mass fraction be 6wt.%~10wt.% when performance most It is good；The too low demercuration adsorbent that is easily caused of the mass fraction of copper chloride produces Cu-lyt. in use, and mass fraction is too It is high chlorination copper crystal occur in adsorbent surface, the oxidation susceptibility of copper chloride can be all affected, the demercuration absorption is affected then The activity of agent.Due to Ce(1-x)ZrxO2If 5min~10min is adsorbable about during powder impregnated in isopyknic copper chloride solution 95% copper chloride, before step S1, can prepare copper chloride solution previously according to the mass fraction of the copper chloride of required load.
Embodiment 1
(1) (preparation method is referring to document to prepare cerium zirconium sosoloid powder with sol-gal process《Zhou et al.Manganese doped CeO2-ZrO2catalyst for elemental mercury oxidation at low temperature.》(Fuel Processing Technology 152,285-293), its molecular formula are Ce0.67Zr0.33O2, The particle size range of powder particle is between 50 μm~100 μm；
(2) 5.64g cerium zirconium sosoloids be impregnated in into 5min in isopyknic 76g/L copper chloride solutions；
(3) in air atmosphere, the cerium zirconium sosoloid that the step (2) is obtained standing and drying 24 under the conditions of 25 DEG C is little Shi Hou, is dried 12 hours in 65 DEG C of baking oven then, obtains the adsorbent that powder 6g loads copper chloride, chlorination in adsorbent The mass fraction of copper is 6%.
(4) These powdered adsorbents are cellular adsorbent through mould extrusion molding, the cellular adsorbent A length of 1200mm, section are square, and the foursquare length of side is 30mm, its front and rear surfaces is announced has 30 × 30 sizes for 8 × The square hole of 8mm, the wall thickness of the square hole is 1mm, as shown in Figure 1.Using the adsorbent as a unit, coal-fired electricity is transported to Factory, after economizer, before cleaner unit, with the 10 μ g/m of concentration of elemental mercury from coal-fired flue gas3, exhaust gas volumn 5000000m3/h。 Adsorbent mounting means is the assembling of multiple units, is primarily determined that as 60 × 60 catalyst elements, therefore catalyst totality Product is defined as 317m3.Two-layer is arranged.
Embodiment 2
Repeat embodiment 1 with described same steps, difference is in the step (4) to pacify honeycomb sorbent agent After being mounted in economizer and cleaner unit.
The adsorbent of embodiment 3-6 is prepared with step same as Example 1, and concrete preparation parameter is as shown in table 1, in table Not listed parameter and method are same as Example 1.
Table 1
Interpretation
Adsorbent prepared by the step of choosing 50mg embodiment 1 (3) carries out adsorption effect-laboratory test.Test temperature For 200 DEG C, smoke components (without chlorine) are N2+ 6%O2+ 12%CO2+800ppmv SO2+ 300ppmvNO+8%H2O+50μg/ m3Hg.Test result shows that, after operation 140 hours, the demercuration efficiency of adsorbent still has 20%.
Adsorbent prepared by the step of alternative takes 50mg embodiments 1 (3) carries out adsorption effect-laboratory test.Test temperature Spend for 200 DEG C, smoke components (low chlorine) are N2+ 6%O2+ 12%CO2+800ppmv SO2+ 300ppmvNO+8%H2O+50μg/ m3Hg+1ppm HCl, after adsorbent runs 210 hours, the demercuration efficiency of adsorbent still has 20%.
Adsorbent prepared by the step of choosing 50mg embodiment 1 (3) carries out adsorption effect-laboratory test.Test temperature For 200 DEG C, smoke components (without chlorine) are N2+ 6%O2+100μg/m3Hg.Test result shows, after operation 2 hours, the present invention In the demercuration efficiency of adsorbent still maintain 80% up to the demercuration efficiency of adsorbent after 95%, 10 hour.
The mass fraction of the copper chloride in adsorbent prepared by embodiment 3-6 is 3wt.%~15wt.%, and empirical tests have Effect similar to Example 1；Wherein, when the mass fraction of copper chloride is 6wt.%~10wt.%, the demercuration effect of adsorbent Rate is optimal.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not to The present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc. are limited, all should be included Within protection scope of the present invention.

Claims (10)

1. a kind of demercuration adsorbent for flue gas, it is characterised in that including the Ce of 85wt.%~97wt.%(1-x)ZrxO2Powder And the copper chloride of 3wt.%~15wt.%, the Ce(1-x)ZrxO2The particle diameter of powder is 20 μm~200 μm, the copper chloride It is carried on the Ce(1-x)ZrxO2Powder surface.
2. demercuration adsorbent as claimed in claim 1, it is characterised in that in the Ce(1-x)ZrxO2In, x is 0~0.5.
3. demercuration adsorbent as claimed in claim 2, it is characterised in that in the Ce(1-x)ZrxO2In, x is 0.3~0.4.
4. demercuration adsorbent as claimed in claim 1, it is characterised in that the demercuration adsorbent include 6wt.%~ The copper chloride of 10wt.%.
5. demercuration adsorbent as claimed in claim 1, it is characterised in that the demercuration adsorbent is cellular or tabular.
6. as described in any one in claim 1-5 demercuration adsorbent preparation method, it is characterised in that including following step Suddenly：
S1. by Ce(1-x)ZrxO2Powder infusion is more than the copper chloride solution 3min of 10g/L~500g/L in concentration, is made described Ce(1-x)ZrxO2The area load copper oxide of powder, and the copper oxide and Ce of the load(1-x)ZrxO2The mass ratio of powder is 3: 97~3:17；
S2. the Ce of copper oxide will be loaded with(1-x)ZrxO2Powder is fully dried, and obtains the demercuration adsorbent.
7. preparation method as claimed in claim 6, it is characterised in that copper chloride solution and Ce in step S1(1-x)ZrxO2 The volume of powder is equal, and the time of the dipping is 5min~10min.
8. preparation method as claimed in claim 6, it is characterised in that the method being fully dried in step S2 is：First More than 24h is kept below 30 DEG C, then in 50 DEG C~75 DEG C of temperature heating 6h~12h.
9. preparation method as claimed in claim 6, it is characterised in that also include step S3 after step S2：By institute State demercuration adsorbent and be compressed to cellular or tabular.
10. application of the demercuration adsorbent as described in any one in claim 1-5 in the demercuration of flue gas.
CN201611119518.2A 2016-12-08 2016-12-08 Mercury removal adsorbent for flue gas as well as preparation method and application thereof Pending CN106669354A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102698753A (en) * 2012-05-15 2012-10-03 中国科学院过程工程研究所 Catalyst for mercury oxidation and preparation method and purpose thereof
CN102716736A (en) * 2012-06-29 2012-10-10 南京工业大学 Composite catalyst capable of depriving nitre and mercury simultaneously and preparation method thereof
CN104492414A (en) * 2014-12-02 2015-04-08 上海华明高纳稀土新材料有限公司 Preparation method of cerium-zirconium based solid solution

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102698753A (en) * 2012-05-15 2012-10-03 中国科学院过程工程研究所 Catalyst for mercury oxidation and preparation method and purpose thereof
CN102716736A (en) * 2012-06-29 2012-10-10 南京工业大学 Composite catalyst capable of depriving nitre and mercury simultaneously and preparation method thereof
CN104492414A (en) * 2014-12-02 2015-04-08 上海华明高纳稀土新材料有限公司 Preparation method of cerium-zirconium based solid solution

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