CN101480605A - Novel activated carbon fiber adsorbing substance as well as preparation method and use thereof - Google Patents
Novel activated carbon fiber adsorbing substance as well as preparation method and use thereof Download PDFInfo
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- CN101480605A CN101480605A CNA2009100953020A CN200910095302A CN101480605A CN 101480605 A CN101480605 A CN 101480605A CN A2009100953020 A CNA2009100953020 A CN A2009100953020A CN 200910095302 A CN200910095302 A CN 200910095302A CN 101480605 A CN101480605 A CN 101480605A
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Abstract
The invention discloses a novel activated carbon fiber adsorbent a preparation method and the application thereof. The activated carbon fiber adsorbent is characterized by carrying MoS2 on the surface of activated carbon fiber. The preparation method comprises the following steps: the activated carbon fiber is used as a carrier, ammonium molybdate is used as a precursor, and deionized water is used as a solvent to be prepared into steeping liquor, wherein the mass ratio of the activated carbon fiber to the ammonium molybdate is 1 : 0.25 to 0.3; the ammonium molybdate is carried in the activated carbon fiber by a wet immersion method, and then, the activated carbon fiber immersed with the ammonium molybdate is heated to 450 to 500 DEG C in inert atmosphere to be oxidized and decomposed to obtain MoO3-activated carbon fiber; and then, the MoO3-activated carbon fiber is heated to 800 to 825 DEG C in Ar/H2S to be sulfurized, and finally, the activated carbon fiber with the surface carried with MoS2 is prepared, i.e. the activated carbon fiber adsorbent is prepared. When the activated carbon fiber adsorbent is used for removing mercury in fume, the effect is good, and the activated carbon fiber adsorbent also has the advantages of simple preparation and easy process control.
Description
(1) technical field
The present invention relates to a kind of novel activated carbon fiber adsorbing substance and its production and application, be specifically related to its application as a kind of mercury-removing adsorbent.
(2) background technology
Mercury is owing to its hypertoxicity, and biological rich long-pending property receives much attention with being difficult to seizure.The mercury of low concentration makes the agriculture underproduction, and the mercury of higher concentration causes crop death.Mercury is transformed into methyl mercury under action of microorganisms.Methyl mercury is a kind of toxicity material stronger than mercury, and its harm that causes is bigger.In a single day mercury enter atmosphere, can be stored for a long time in environment and cause long-term pollution problem.Mercury in the atmospheric environment is very most of from human activity.Wherein the mercury of coal combustion and waste incineration generation accounts for the overwhelming majority.
Present smoke pollution control device can remove divalence mercury preferably and solid granulates adheres to mercury, but not obvious to the removal effect of nonvalent mercury.Sorbent injection has become the most promising at present active mercury emissions control research direction in conjunction with electrostatic precipitator or sack cleaner method.The technology of existing control mercury emissions: washed coal removal of mercury technology, sorbent injection technology, conventional pollutant control removal of mercury technology etc. still are confined to conceptual phase.Do not have in these technology a kind ofly can from waste gas, remove mercury, particularly nonvalent mercury fully.
Therefore, be necessary to develop a kind of more effectively mercury-removing adsorbent.
(3) summary of the invention
First technical problem that the present invention will solve provides a kind of novel, activated carbon fiber adsorbing substance efficiently.
Activated carbon fiber adsorbing substance of the present invention is at the NACF area load MoS to be arranged
2Described activated carbon fiber adsorbing substance is prepared as follows and obtains: be carrier with the NACF, with the ammonium heptamolybdate is presoma, deionized water is that solvent is made into maceration extract, the mass ratio of described NACF and ammonium heptamolybdate is 1:0.25～0.3, adopt the wet impregnation method that ammonium heptamolybdate is carried in the described NACF, the NACF that will be impregnated with ammonium heptamolybdate again is heated to 450～500 ℃ of oxidation Decomposition under inert atmosphere, promptly get MoO
3-NACF, and then at Ar/H
2Under the S atmosphere, be heated to 800～825 ℃ and vulcanize, making area load has MoS
2NACF, be described activated carbon fiber adsorbing substance.
Second technical problem that the present invention will solve provides a kind of method for preparing above-mentioned activated carbon fiber adsorbing substance.
The technical solution used in the present invention is as follows:
A kind of preparation method of activated carbon fiber adsorbing substance comprises the steps:
A) get NACF, fully flood, obtain being impregnated with the NACF of ammonium heptamolybdate with the ammonium heptamolybdate aqueous solution; The mass ratio of described NACF and ammonium heptamolybdate is 1:0.25～0.3;
B) NACF that will be impregnated with ammonium heptamolybdate is heated to 450～500 ℃ under inert atmosphere, carries out oxidation Decomposition, makes MoO
3-NACF;
C) at Ar/H
2Under the S atmosphere, with MoO
3-NACF is heated to 800～825 ℃ of sulfurations, and making area load has MoS
2NACF, be described activated carbon fiber adsorbing substance.
Below above-mentioned preparation method is specified.
In the step a), the kind that described NACF is commonly used has viscose glue base class, polyacrylonitrile base class, phenolic aldehyde base class and pitch base class, the preferred viscose-based active carbon fiber of the present invention.
In dipping process, improve temperature and help to improve dipping efficient, dipping of the present invention preferably carried out 24～48 hours under 40～50 ℃ of temperature.
Among the present invention, the preferred 4～4.8mg/ml of the concentration of described Ammoniun Heptamolybdate Solution.
After described active carbon fibre Wesy Ammoniun Heptamolybdate Solution fully floods, ammonium heptamolybdate enters in the micropore of NACF, but also can residually there be ammonium heptamolybdate on its surface, might cause adsorbing the duct stops up, influence absorption property, so preferably wash repeatedly and removed, and then carry out the operation of step b) with deionized water.
In the step b), the preferred Ar gas of described inert gas is generally carried out in the heated oxide decomposition that is impregnated with the NACF of ammonium heptamolybdate of the present invention in tube furnace.Described oxidation Decomposition is recommended in 450～500 ℃ and carried out 3～4 hours.In the heated oxide decomposable process, can produce NH
3Waste gas generally needs the configuration dilute hydrochloric acid solution so that absorb the tail gas (NH that produces when decomposing
3Waste gas).
In the step c), sulfuration of the present invention is recommended to carry out according to following steps: with MoO
3-NACF places tube furnace, at Ar/H
2Under the S atmosphere, control described Ar/H
2H in the S atmosphere
2The volume ratio of S and Ar is 1:19～49, with MoO
3-NACF is heated to 800～825 ℃ of sulfurations 1～3.5 hour, and making area load has MoS
2NACF.In the sulfidation, can adopt diluted sodium hydroxide solution to absorb the H of afterbody
2S waste gas.
The 3rd technical problem that the present invention will solve is that described activated carbon fiber adsorbing substance is used as mercury-removing adsorbent, removes mercury from mercury fume, nonvalent mercury especially wherein.
Activated carbon fiber adsorbing substance of the present invention is applicable to that mercury concentration is 0.01～100mg/m in the flue gas stream
3Scope in carry out mercury removal, can obtain very high removal of mercury efficient; Also be suitable for very wide flue-gas temperature scope,, be preferably 100～200 ℃ from environment temperature to 300 ℃; Both be applicable to that the better simply flue gas stream of gas componant was as Hg, H
2O, N
2And CO
2, also be applicable to the flue gas stream of gas component complexity as comprise O
2, CO
2, SO
2, NO, NO
2, HCl, H
2O and N
2Flue gas stream etc. multiple sour gas can obtain good mercury removal effect.
Under each implementation condition, activated carbon fiber adsorbing substance of the present invention all is better than undressed NACF far away to the absorption property of mercury.In the absorption starting stage, can make Hg
0Concentration is dropped rapidly to 0 μ g/m
3, keep the long period at this concentration level subsequently, and reach capacity far away, have very strong mercury absorption property.The saturated extent of adsorption of activated carbon fiber adsorbing substance of the present invention can reach the orders of magnitude up to ten thousand (μ g Hg as calculated
0/ g adsorbent), be a kind of high-efficiency adsorbent that removes mercury in the flue gas.
Compared with prior art, beneficial effect of the present invention is embodied in:
1) activated carbon fiber adsorbing substance of the present invention, with the NACF of function admirable as carrier, at its area load the MoS of nanoscale
2Molybdenum bisuphide (MoS
2) because of having performances such as good light, electricity, lubricated, catalysis, people's attention extremely always.So when the NACF area load MoS of nanoscale
2After it is further promoted on many performances, show highlightedly: adsorption capacity is stronger, the reactivity height.Therefore, activated carbon fiber adsorbing substance of the present invention has shown good effect when using as the adsorbent that removes the mercury in the flue gas.
2) preparation method of activated carbon fiber adsorbing substance of the present invention is simple, realizes easily.Use wet impregnation method to NACF, utilizes the characteristic of ammonium heptamolybdate pyrolytic to make MoO the ammonium heptamolybdate direct impregnation
3-NACF makes MoS after the sulfuration again
2-NACF.Produce MoS with mentioning in other documents
2Method (as oxide or the molybdenum carbonyl and S reaction, sulfide thermal decomposition etc. of amino-compound reduction molybdenum trioxide, molybdenum) compare, this preparation method is convenient direct, whole chemical treating process is easy to control.
(4) description of drawings
Fig. 1 is the sem photograph of activated carbon fiber adsorbing substance of the present invention.
Fig. 2 is the energy spectrum analysis figure of activated carbon fiber adsorbing substance of the present invention.
Fig. 3 is N
2The adsorption curve of activated carbon fiber adsorbing substance of the present invention under the atmosphere.
Fig. 4 is N
2The adsorption curve of original activity charcoal fiber under the atmosphere.
Fig. 5 is N
2MoO under the atmosphere
3The adsorption curve of-activated carbon fiber adsorbing substance.
Fig. 6 is the schematic diagram of the applied flue gas adsorbent equipment of the present invention.
(5) specific embodiment
Below in conjunction with accompanying drawing the present invention is further described.
Embodiment one
Take by weighing the 1g ammonium heptamolybdate and place beaker, add deionized water and stirring and make its dissolving.Ammoniun Heptamolybdate Solution is moved into the 250ml volumetric flask, and constant volume promptly makes the Ammoniun Heptamolybdate Solution that concentration is 4mg/ml.(specific area is 1000m to get the 4g NACF
2The viscose-based active carbon fiber of/g) places the brown wide-mouth bottle of 250ml, add the 250ml Ammoniun Heptamolybdate Solution.Under 40 ℃ of water bath condition, the absorption dipping washed NACF repeatedly with deionized water after 24 hours.Be placed on then in the porcelain boat,, under the Ar atmosphere (air velocity 200ml/min), added thermal decomposition 3 hours, promptly make area load molybdenum trioxide (MoO in 450 ℃ in tube furnace
3) NACF.In adding thermal decomposition process, the tail gas (NH that produces when needing the configuration dilute hydrochloric acid solution to decompose to absorb
3Waste gas).
Get 0.5g MoO
3-NACF places in the porcelain boat, at 800 ℃ in tube furnace, Ar/H
2S (Ar:H
2S=49:1) (air velocity 200ml/min) under the atmosphere, baking 1.5 hours promptly makes MoS on the area load
2Activated carbon fiber adsorbing substance.In the sulfidation, adopt diluted sodium hydroxide solution to absorb the H of afterbody
2S waste gas.
Embodiment two
Take by weighing the 1g ammonium heptamolybdate and place beaker, add deionized water and stirring and make its dissolving.Ammoniun Heptamolybdate Solution is moved into the 250ml volumetric flask, and constant volume promptly makes the Ammoniun Heptamolybdate Solution that concentration is 4mg/ml.(specific area is 1000m to get the 4g NACF
2The viscose-based active carbon fiber of/g) places the brown wide-mouth bottle of 250ml, add the 250ml Ammoniun Heptamolybdate Solution.Under 45 ℃ of water bath condition, standing adsorption is washed NACF repeatedly with deionized water after about 24 hours.Be placed on then in the porcelain boat,, under the Ar atmosphere (air velocity 200ml/min), added thermal decomposition 3.5 hours, promptly make area load molybdenum trioxide (MoO in 450 ℃ in tube furnace
3) NACF.In adding thermal decomposition process, the tail gas (NH that produces when needing the configuration dilute hydrochloric acid solution to decompose to absorb
3Waste gas).
Get 0.5g MoO
3-NACF places in the porcelain boat, at 820 ℃ in tube furnace, Ar/H
2Under S (Ar:H2S=19:1) atmosphere (air velocity 100ml/min), about 1 hour of baking promptly makes MoS on the area load
2Activated carbon fiber adsorbing substance.In the sulfidation, adopt diluted sodium hydroxide solution to absorb the H of afterbody
2S waste gas.
Embodiment three
Take by weighing the 10g ammonium heptamolybdate and place beaker, add deionized water and stirring and make its dissolving, compound concentration is the Ammoniun Heptamolybdate Solution of 4mg/ml.(specific area is 1000m to get the 8g NACF
2The viscose-based active carbon fiber of/g) places the brown wide-mouth bottle of 500ml, add the 500ml Ammoniun Heptamolybdate Solution.Under 50 ℃ of water bath condition, standing adsorption was washed NACF repeatedly with deionized water after 48 hours.Be placed on then in the porcelain boat,, under the Ar atmosphere (air velocity 200ml/min), added thermal decomposition 4 hours, promptly make area load molybdenum trioxide (MoO in 500 ℃ in tube furnace
3) NACF.In adding thermal decomposition process, the tail gas (NH that produces when needing the configuration dilute hydrochloric acid solution to decompose to absorb
3Waste gas).
Get 5g MoO
3-NACF places in the porcelain boat, at 825 ℃ in tube furnace, Ar/H
2S (Ar:H
2S=49:1) (air velocity 1000ml/min) under the atmosphere, baking 3.5 hours promptly makes MoS on the area load
2Activated carbon fiber adsorbing substance.In the sulfidation, adopt diluted sodium hydroxide solution to absorb the H of afterbody
2S waste gas.
Embodiment four
Taking by weighing 10g ammonium heptamolybdate compound concentration is the Ammoniun Heptamolybdate Solution of 4mg/ml.(specific area is 1000m to get the 8g NACF
2The viscose-based active carbon fiber of/g) places the brown wide-mouth bottle of 500ml, add the 500ml Ammoniun Heptamolybdate Solution.Under 50 ℃ of water bath condition, standing adsorption was washed NACF repeatedly with deionized water after 48 hours.Be placed on then in the porcelain boat,, under the Ar atmosphere (air velocity 200ml/min), added thermal decomposition 4 hours, promptly make area load molybdenum trioxide (MoO in 500 ℃ in tube furnace
3) NACF.In adding thermal decomposition process, the tail gas (NH that produces when needing the configuration dilute hydrochloric acid solution to decompose to absorb
3Waste gas).
Get 5g MoO
3-NACF places in the porcelain boat, at 825 ℃ in tube furnace, Ar/H
2S (Ar:H
2S=19:1) (air velocity 1000ml/min) under the atmosphere, about 1.5 hours of baking promptly makes MoS on the area load
2Activated carbon fiber adsorbing substance.In the sulfidation, adopt diluted sodium hydroxide solution to absorb the H of afterbody
2S waste gas.
Fig. 1 has MoS for area load
2The sem photograph of activated carbon fiber adsorbing substance, MoS as can be known
2Mainly with the graininess of nanoscale attached on the NACF surface, size distribution is more even.Fig. 2 has MoS for area load
2The energy spectrum analysis figure of activated carbon fiber adsorbing substance, table 2 has MoS for area load
2The elementary analysis of activated carbon fiber adsorbing substance contain scale, Mo element and S constituent content are higher as can be known, the NACF area load has been described a certain amount of MoS
2
The present invention places a kind of flue gas mercury adsorbent equipment with Application Example, comparative example one, comparative example two said activated carbon fiber adsorbing substances, feeds mercury fume, makes activated carbon fiber adsorbing substance fully adsorb mercury (adsorption time is seen each embodiment) in the mercury fume.
Flue gas mercury adsorbent equipment of the present invention, as Fig. 6, be meshing with each other by upper glass pipe 1 and lower-glass pipe 2 and constitute, the air inlet 11 of described upper glass pipe 1 and the gas outlet 21 of lower-glass pipe 2 all present bundle mouthful shape, be provided with hollow out overhead gage 3 in the described upper glass pipe 1, be provided with hollow out lower baffle plate 4 in the described lower-glass pipe 2, the below of described overhead gage 3 and lower baffle plate 4 tops all are provided with dismountable mineral wool layer 5, leave the cavity 6 that can place solid absorbent between described overhead gage 3 and the lower baffle plate 4.The outer wall of described upper glass pipe 1 and lower-glass pipe 2 all is provided with bossed hook 7.The port one 2 of described upper glass pipe 1 inserts the port 22 of described lower-glass pipe 2, and described port contact surface has the frosted layer, makes the engagement of port junction tightr like this, prevents gas leakage.Detachable upper and lower glass tube 1,2 in the process of the test is changed mineral wool layer 5 or is loaded adsorbent layer, to constitute fixed adsorption bed.Upper glass pipe and lower-glass bore are 20mm, and length is 70mm, and described overhead gage or lower baffle plate are that 4 thickness are the fan-shaped quartz glass plate of 3～4mm, radial being evenly arranged in the glass tube, and described overhead gage is 110mm to the distance of lower baffle plate.Described overhead gage or lower baffle plate are fixed on the bundle mouth 15mm～20mm place apart from the bundle mouth of upper glass pipe or lower-glass pipe.Cotton layer of the cotton layer of new upper glass and lower-glass arranged in the top of the below of overhead gage or lower baffle plate during use, the thickness 25mm that respectively does for oneself.
Application Example
Get the described area load of 0.015g MoS is arranged
2Activated carbon fiber adsorbing substance, at N
2Under the atmosphere, the mercury fume flow is 1L/min, initial Hg
0Concentration is 67.3 μ g/m
3, 130 ℃ of adsorption temps carry out Hg
0Adsorption experiment.Adsorption curve is adsorbing starting stage, Hg as shown in Figure 3
0Concentration is from 67.3 μ g/m
3Be dropped rapidly to 0 μ g/m
3, subsequently at 0 μ g/m
3Concentration level vibrates up and down.In 41 hours adsorption processes, Hg
0Concentration slowly rises to 5 μ g/m
3Near, MoS
2-carbon fiber adsorption and catalytic combustion amount does not reach capacity yet, also has very strong mercury absorption property.MoS as calculated
2The saturated extent of adsorption of-NACF can reach the orders of magnitude up to ten thousand (μ gHg
0/ g adsorbent), be a kind of high-efficiency adsorbent that removes nonvalent mercury in the flue gas.
Comparative example one
Get 0.015g original activity charcoal fiber (without chemical impregnation) and compare test, at N
2Under the atmosphere, the mercury fume flow is 1L/min, initial Hg
0Concentration is 114 μ g/m
3, adsorption curve as shown in Figure 4.The absorption starting stage, Hg
0Concentration is from 114 μ g/m
3Descend rapidly, near 0 μ g/m
3, slowly rise again subsequently, through about 1 hour absorption, original activity charcoal fiber is penetrated, and as seen it has certain absorption property to nonvalent mercury, but effect is general.From the unit of each sample of sorbent of table 2 absorption scale as can be known, MoS
2-NACF is compared with original activity charcoal fiber, and its mercury absorption property obtains to promote significantly.Therefore, MoS
2-NACF is a kind of efficient mercury absorbent.
Comparative example two
Get the described MoO of 0.015g
3-NACF compares test, under N2 atmosphere, and mercury fume flow 1L/min, initial Hg
0Concentration is 76.1 μ g/m
3, adsorption curve as shown in Figure 5.After the absorption beginning, Hg
0Concentration is from 76.1ug/m
3Drop to 46.5ug/m
3, slowly rise subsequently, through about 2.5 hours absorption, Hg
0The amplitude that concentration is gone up is not very big, still has certain adsorption capacity.Compare MoO with original activity charcoal fiber
3-NACF concentration decline degree when initial adsorption is not very big, but its absorption duration is long than original activity charcoal fiber, thereby, MoO
3The mercury absorption property of-NACF promotes to some extent than original activity charcoal fiber, but with sulfuration back sample MoS
2-NACF is compared and there is a big difference.In addition, the unit adsorbance data from table 2 more also can obtain same conclusion.Therefore, MoS
2-NACF is a kind of mercury absorbent efficiently.
Table 1 MoS
2The constituent content table of-NACF
| Element | C | N | O | S | Mo | Other |
| Content (%) | 56.97 | 4.53 | 11.51 | 9.20 | 17.78 | 0.01 |
The unit absorption scale of each sample of sorbent of table 2
| Adsorbent | Smoke components | Unit adsorbance (μ g/g) | Conversion unit adsorbance (μ g/g) |
| Original activity charcoal fiber | N 2 | 172.13 | 166.09 |
| MoS 2-NACF | N 2 | 9892.67 | 16871.2 |
| MoO 3-NACF | N 2 | 211.49 | 302.13 |
Annotate: conversion unit adsorbance---because that the infiltration rate of mercury pipe is subjected to permeating the influence of temperature and carrier gas air-flow is bigger, therefore the mercury initial concentration of each sample absorption difference to some extent, for under same initial concentration levels, comparing the adsorption capacity of each adsorbent, all the unit absorption value of each sample is converted 110 μ g/m
3Initial mercury concentration level.
Claims (10)
1, a kind of activated carbon fiber adsorbing substance is characterized in that described activated carbon fiber adsorbing substance is at the NACF area load MoS to be arranged
2Described activated carbon fiber adsorbing substance is prepared as follows: be carrier with the NACF, with the ammonium heptamolybdate is presoma, deionized water is that solvent is made into maceration extract, the mass ratio of described NACF and ammonium heptamolybdate is 1:0.25～0.3, adopt the wet impregnation method that ammonium heptamolybdate is carried in the described NACF, the NACF that will be impregnated with ammonium heptamolybdate again is heated to 450～500 ℃ of oxidation Decomposition under inert atmosphere, promptly get MoO
3-NACF, and then at Ar/H
2Under the S atmosphere, be heated to 800～825 ℃ and vulcanize, making area load has MoS
2NACF, be described activated carbon fiber adsorbing substance.
2, a kind of preparation method of activated carbon fiber adsorbing substance as claimed in claim 1, described preparation method comprises the steps:
A) get NACF, fully flood, obtain being impregnated with the NACF of ammonium heptamolybdate with the ammonium heptamolybdate aqueous solution; The mass ratio of described NACF and ammonium heptamolybdate is 1:0.25～0.3;
B) NACF that will be impregnated with ammonium heptamolybdate is heated to 450～500 ℃ under inert atmosphere, carries out oxidation Decomposition, makes MoO
3-NACF;
C) at Ar/H
2Under the S atmosphere, with MoO
3-NACF is heated to 800～825 ℃ of sulfurations, and making area load has MoS
2NACF, be described activated carbon fiber adsorbing substance.
3, the preparation method of activated carbon fiber adsorbing substance as claimed in claim 2 is characterized in that the described dipping of step a) is to carry out 24～48 hours under 40～50 ℃ of temperature.
4, the preparation method of activated carbon fiber adsorbing substance as claimed in claim 2, the concentration that it is characterized in that the described ammonium heptamolybdate aqueous solution of step a) is at 4～4.8mg/ml.
5, as the preparation method of the described activated carbon fiber adsorbing substance of one of claim 2～4, it is characterized in that the described active carbon fibre of step a) Wesy Ammoniun Heptamolybdate Solution fully floods after, wash repeatedly with deionized water, and then carry out the operation of step b).
6, the preparation method of activated carbon fiber adsorbing substance as claimed in claim 2 is characterized in that the described inert gas of step b) is an Ar gas.
7, the preparation method of activated carbon fiber adsorbing substance as claimed in claim 2, the reaction time that it is characterized in that the described oxidation Decomposition of step b) is 3～4 hours.
8, the preparation method of activated carbon fiber adsorbing substance as claimed in claim 2 is characterized in that the described sulfuration of step c) carries out according to following steps: with MoO
3-NACF places tube furnace, at Ar/H
2Under the S atmosphere, control described Ar/H
2H in the S atmosphere
2The volume ratio of S and Ar is 1:19～49, with MoO
3-NACF is heated to 800～825 ℃ of sulfurations 1～3.5 hour, and making area load has MoS
2NACF.
9, activated carbon fiber adsorbing substance as claimed in claim 1 is as the application of mercury-removing adsorbent.
10, application as claimed in claim 9 is characterized in that described mercury is nonvalent mercury.
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| US8034741B2 (en) * | 2005-11-09 | 2011-10-11 | Gore Enterprise Holdings, Inc. | Capture of mercury from a gaseous mixture containing mercury |
| JP5094468B2 (en) * | 2007-03-01 | 2012-12-12 | 日本エンバイロケミカルズ株式会社 | Method for removing mercury vapor from gas |
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