CN104014304A - Nitric acid modified activated carbon adsorbent for demercuration of flue gas, and preparation method and application thereof - Google Patents
Nitric acid modified activated carbon adsorbent for demercuration of flue gas, and preparation method and application thereof Download PDFInfo
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- CN104014304A CN104014304A CN201410214670.3A CN201410214670A CN104014304A CN 104014304 A CN104014304 A CN 104014304A CN 201410214670 A CN201410214670 A CN 201410214670A CN 104014304 A CN104014304 A CN 104014304A
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Abstract
The invention relates to a nitric acid modified activated carbon adsorbent for demercuration of a flue gas, and a preparation method and application thereof. The preparation method comprises the steps of washing activated carbon in a certain size range clean with distilled water, drying for use; preparing a certain concentration of a nitric acid modified solution; then impregnating the activated carbon by using the solution; and finally washing a filtrate and drying to obtain the nitric acid modified activated carbon adsorbent used for the demercuration. The nitric acid modified activated carbon adsorbent takes use of the characteristic that nitric acid can increase surface functional groups of the activated carbon, so that mercury is captured when a mercury-containing flue gas component enters a porous structure of the activated carbon. The nitric acid modified activated carbon is an efficient demercuration adsorbent specialized forflue gas injection demercuration of power plants, industrial boilers and industrial furnaces; operation and the preparation processes have the advantages of low energy consumption, simple operations and low cost; and mercury adsorption capacity of the modified activated carbon is greatly improved, thereby effectively controlling mercury in the coal-fired flue gas.
Description
Technical field
The invention belongs to flue gas pollutant control field, relate generally to a kind of method of applying Carbon Materials adsorbing and removing mercury in flue gas, be specifically related to a kind of Nitric Acid Modified acticarbon, Preparation Method And The Use for flue gas demercuration.
Background technology
China is big coal country, also be coal-fired big country, coal in energy resource structure proportion up to 75%, the annual coal consumption amount of China is 2,000,000,000 tons of left and right, wherein more than 70% be used as coal fired power generation, in coal combustion process, can produce a large amount of pollutants, and micro heavy mercury has persistence, easily migration and feature such as height bioconcentration etc., the mankind and ecological environment are produced to greatly harm.
In coal-fired flue-gas, diffuse into airborne mercury and have three kinds of existence forms: element mercury (Hg
0), oxidation state mercury (Hg
2+), particle mercury (Hg
p).Wherein, Hg
2+can remove by wet flue gas desulfurizer because it is soluble in water; Hg
peasily caught and removed by electrostatic precipitator or sack cleaner; And Hg
0due to its high volatile volatile be insoluble in water and become the Focal point and difficult point of current mercury pollution control.The mercury phase specific concentration that the mercury that coal burning produces and city garbage incinerator discharge is lower, and its quantity and scale become the most important artificial source of mercury emissions, have therefore more aggravated the difficulty of its improvement.
The control technology of coal-fired flue-gas mercury can be divided into demercuration and the rear demercuration technology of burning in the front demercuration of burning, burning.Demercuration technology after the more burning of at present research, is mainly mercury adsorption technology, and active carbon is considered in coal-fired flue-gas one of the most effective mercury absorbent because it has huge specific area and abundant surface functional group, enjoys domestic and international expert's concern.But active carbon cost is slightly high, will certainly limit its extensive use, therefore need to find suitable method of modifying, prepare the active carbon of high adsorption activity, reduce active carbon use cost.
CN103223330A discloses a kind of application H
2o
2the method of modified activated carbon adsorbing and removing mercury, said method comprising the steps of: (1) by wood substance grain active carbon, after chlorohydric acid pickling, distilled water washing, and dry for standby; (2) press mass volume ratio 6g:15-10ml, get the H that active carbon and mass percent concentration are 25-30%
2o
2at 50-70 DEG C, heat 2-4h, afterwards ultrasonic 20-40min; (3) after having left standstill, filter, dry, washing, dry again, obtains the dedicated modified active carbon of demercuration afterwards.This kind of method changed the pore-size distribution of active carbon and the kind of surface functional group and content by heat modification and supersonic modifying, and the highest mercury adsorption capacity of the modified activated carbon of preparing is 1.5 times of unmodified active carbon.
CN101474551A discloses a kind of sulfur loading active carbon for flue gas demercuration and preparation method thereof, said method comprising the steps of: (1) is after 20-40 object active carbon washes by granularity, dry for standby; (2) container that fills simple substance sulphur is placed in to the bottom of thermoprecipitation stove, active carbon is placed on the second container at thermoprecipitation stove middle part, and sealing, passes into 1-2L/min High Purity Nitrogen 30-40min, discharges the air in thermoprecipitation stove; Adjust N
2flow 0.5L/min, is warming up to 400-600 DEG C, and after being incubated 50-90 minute, stops heating; Adjust N
2flow 1-2L/min, with the furnace temperature of heat of cooling precipitation stove, makes above-mentioned active carbon.Described method loads on active carbon sulphur by thermal precipitator method, and the active carbon sulfur content after load is high, and is evenly distributed on active carbon, and this active carbon pore volume and pore-size distribution still have advantages of active carbon.
CN102515162A discloses a kind of activated carbon from activated sludge and preparation method thereof, said method comprising the steps of: (1) taking common agricultural crop straw as raw material, the ZnCl that is 20%-50% by concentration
2dipping 20-30h; (2) after dipping, adopting nitrogen protection, is carbonization 1.5h-3h under the condition of 400-700 DEG C in temperature, naturally cooling after taking out; (3) the salt pickling with 5%-15% by active carbon after carbonization,,, dries and grinds and make activated carbon from activated sludge and with Filter paper filtering to neutral with distilled water rinsing.Described method has been prepared chlorine modified activated carbon for the removing of gas mercury by infusion process, and the ability of the charcoal absorption mercury of preparing is improved.
CN101850240A discloses the preparation method of a kind of year bromine active carbon, said method comprising the steps of: common active carbon adds after bromine reaction device internal burden bromine in drum-type, and screening obtains.Described method bromine load capacity >=10%, mercury adsorption capacity >=0.2mg/g after load.
Domestic a lot of scholar has done a certain amount of research to activated carbon modified, but also in the starting stage, and mainly concentrate on sulphur, halogen modified research, and carry out activated carbon modified cost lower than carry out modification with sulphur, halogen with nitric acid, thereby may there is more wide application prospect.
Summary of the invention
One of the object of the invention is to provide a kind of Nitric Acid Modified acticarbon removing that is applied to mercury in flue gas, and this adsorbent has suitable demercuration efficiency, when outlet mercury concentration reach entrance mercury concentration 90% time, the adsorbance of mercury is 222ug/g.
The mixing of one or several that the active carbon for mercury absorption of the present invention is domestic commercially available cocoanut active charcoal, coal mass active carbon, active fruit shell carbon, bamboo granular activated carbon or Powdered Activated Carbon; preferably cocoanut active charcoal and/or active fruit shell carbon, further preferred cocoanut active charcoal.Described adsorbent makes through infusion process.
Two of object of the present invention is to provide a kind of described method of modifying for activated carbon used for flue gas demercuration adsorbent, and described method is nitric acid infusion process.Infusion process refers to active carbon is placed in to the liquid or the gas that contain active component, makes active component enter the preparation method of the adsorbent of carrier inside through certain hour.
The present invention is specifically by the following technical solutions:
For a preparation method for the Nitric Acid Modified acticarbon of flue gas demercuration, said method comprising the steps of:
1) preparation molar concentration is >=salpeter solution of 1mol/L, mixes and leaves standstill clarification;
2) active carbon is impregnated into step 1) in described salpeter solution, ultrasonic concussion 0.5～4h; Then make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas through washing, oven dry.
Described active carbon is the mixture of a kind of in cocoanut active charcoal, coal mass active carbon, active fruit shell carbon, bamboo granular activated carbon or Powdered Activated Carbon or at least two kinds, preferably cocoanut active charcoal and/or active fruit shell carbon; Further preferred cocoanut active charcoal.Typical case but non-limitative example comprise: cocoanut active charcoal; coal mass active carbon; bamboo granular activated carbon; Powdered Activated Carbon, the combination of active fruit shell carbon and bamboo granular activated carbon, the combination of coal mass active carbon and Powdered Activated Carbon; the combination of cocoanut active charcoal, active fruit shell carbon and Powdered Activated Carbon; the combination of coal mass active carbon, active fruit shell carbon and bamboo granular activated carbon, the combination of cocoanut active charcoal, coal mass active carbon, active fruit shell carbon or Powdered Activated Carbon etc., all can be used for implementing the present invention.
Infusion process is prepared in the process of adsorbent, and functional group's kind of activated carbon surface and quantity can be subject to the impact of concentration of nitric acid.Dipping concentration is too low, and functional group's load capacity of activated carbon surface is low and inhomogeneous; Dipping concentration is too high, and the pore passage structure of activated carbon surface can be subject to serious destruction, and the selection of therefore load concentration is extremely important.Molar concentration >=the 1mol/L of the described salpeter solution of step (1), for example: 1mol/L, 1.5mol/L, 2mol/L, 2.5mol/L, 3mol/L, 6mol/L, 7mol/L, 8mol/L etc., preferably >=3mol/L, more preferably 5～8mol/L, most preferably 6mol/L.
Step 2) particle diameter of described active carbon is 20～100 orders, for example: 20～30 orders, 20～40 orders, 30～50 orders, 50～60 orders, 50～90 orders, 80～90 orders, 60～90 orders, 30～80 orders, 40～90 orders etc., preferably 30～90 orders, further preferred 40～80 orders.
Described active carbon and salpeter solution volume ratio are 1:1～5, for example: 1:1,1:1.2,1:1.5,1:2,1:3.5,1:4.5,1:5 etc., further preferred 1:1～1:2, most preferably 1:1.
Described ultrasonic temperature is 25～100 DEG C, for example: 25 DEG C, 28 DEG C, 32 DEG C, 36 DEG C, 50 DEG C, 68 DEG C, 92 DEG C, 100 DEG C etc., preferably 25～60 DEG C, further preferably 25～40 DEG C, most preferably 25 DEG C.
Described supersonic frequency is 40KHz.
Described ultrasonic power is 120～300W, as 120W, 130W, 140W, 160W, 200W, 220W, 250W, 290W, 300W etc., preferably 120～220W, and further preferably 120～180W, most preferably 150W.
In ultrasonic concussion process, maceration extract progressively spreads to inside from active carbon outside, and therefore, dipping needs the process of a balance, and then dip time has determined homogeneity and the maximum functional group load capacity of modification functional group.In the described ultrasonic cleaning machine of step (2), the concussion time is 0.5～4h, for example: 0.1h, 0.3h, 0.5h, 1h, 2h, 2.5h, 3h, 3.6h, 4h etc., preferably 0.5～2h, further preferably 0.5～1h, most preferably 1h.
Step 2) described washing methods is that to use distilled water active carbon to the pH value of filtrate of repeatedly cleaning after modification be 7.
The described bake out temperature of step (2) is at least 60 DEG C, for example: 60 DEG C, 65 DEG C, 78 DEG C, 85 DEG C, 90 DEG C, 105 DEG C, 110 DEG C etc., preferably at least 80 DEG C, more preferably 110 DEG C.
Described drying time is at least 8h, and such as 8.1h, 8.2h, 8.5h, 9h, 25h, 29h, 31h, 31.5h, 31.9h, 32.3h, 33.5h, 37.2h etc., be preferably 8～24h, more preferably 12～24h, most preferably 15h.
For a preparation method for the Nitric Acid Modified acticarbon of flue gas demercuration, specifically comprise the following steps:
1) salpeter solution of preparation molar concentration >=1mol/L, fully mixes and leaves standstill clarification;
2) be 1:1～5 according to the volume ratio of active carbon and salpeter solution, be that 20～100 object active carbons are impregnated in above-mentioned salpeter solution by the order scope of counting, be 25～100 DEG C in temperature, frequency is 40KHz, in the ultrasonic cleaning machine that power is 120～300W, shakes 0.5～4h; Then use distilled water repeatedly to clean after active carbon to the pH value of filtrate after modification is 7, be placed in drying box and at least 60 DEG C, dry at least 8h, make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas.
As the most preferred technical scheme of the present invention, said method comprising the steps of:
1) salpeter solution that preparation molar concentration is 6mol/L, fully mixes and leaves standstill clarification;
2) being 1:1 according to the volume ratio of active carbon and salpeter solution, is that 40～80 object active carbons are impregnated in above-mentioned salpeter solution by the order scope of counting, and is 25 DEG C in temperature, and frequency is 40KHz, and power is to shake 1h in 150W ultrasonic cleaning machine; Then wash, dry and make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas.
A kind of Nitric Acid Modified acticarbon, described adsorbent prepares by method as above.Described Nitric Acid Modified acticarbon is applied in power station, Industrial Boiler, industrial furnace smoke injection demercuration technology.
The present invention is intended to nitric acid impregnation process active carbon, to improve the pore property of original activity charcoal and the kind of surface functional group and distribution, to improve the ability of its adsorbing and removing Mercury In Coal Combustion Flue Gas.
Compared with prior art scheme, the present invention has following beneficial effect:
1) the present invention is flooded modification with certain density salpeter solution to original activity charcoal, by changing the pore property of original activity charcoal and kind and the distribution of surface functional group, improve the ability of its adsorbing and removing Mercury In Coal Combustion Flue Gas, when outlet mercury concentration reach entrance mercury concentration 90% time, the adsorbance of mercury is 222ug/g.
2) nitric acid in the present invention dipping modified activated carbon preparation method simple, be easy to preparation, with low cost, demercuration ability is improved.By the activated carbon application after Nitric Acid Modified in the consumption that can reduce active carbon that removes of Mercury In Coal Combustion Flue Gas, thereby reduce the input cost of active carbon, and then reduce operating cost, therefore there is the space of wide application and development.
Brief description of the drawings
Fig. 1 is the activity rating result figure that embodiment 5 is original, modification obtains acticarbon removes mercury.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, does not represent or limit the scope of the present invention, and protection scope of the present invention is as the criterion with claims.
Detailed description of the invention
Further illustrate technical scheme of the present invention below in conjunction with accompanying drawing and by detailed description of the invention.
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
In the present invention, preparing modified activated carbon salpeter solution used is that company of Beijing Chemical Plant produces, and analyzes pure.
Embodiment 1
For a preparation method for the Nitric Acid Modified acticarbon of flue gas demercuration, specifically comprise the following steps:
1) salpeter solution that preparation molar concentration is 1mol/L, fully mixes and leaves standstill clarification;
2) being 1:1 according to the volume ratio of active carbon and salpeter solution, is that the bamboo granular activated carbon of 20～100 object is impregnated in above-mentioned salpeter solution by the order scope of counting, and is 25 DEG C in temperature, and frequency is 40KHz, in the ultrasonic cleaning machine that power is 120W, shakes 4h; Then use distilled water repeatedly to clean after active carbon to the pH value of filtrate after modification is 7, be placed in drying box and dry 8h at 60 DEG C, make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas.
Embodiment 2
For a preparation method for the Nitric Acid Modified acticarbon of flue gas demercuration, specifically comprise the following steps:
1) salpeter solution that preparation molar concentration is 3mol/L, fully mixes and leaves standstill clarification;
2) being 1:5 according to the volume ratio of active carbon and salpeter solution, is that 30～90 object Powdered Activated Carbons are impregnated in above-mentioned salpeter solution by the order scope of counting, and is 100 DEG C in temperature, and frequency is 40KHz, in the ultrasonic cleaning machine that power is 300W, shakes 0.5h; Then use distilled water repeatedly to clean after active carbon to the pH value of filtrate after modification is 7, be placed in drying box and dry 15h at 80 DEG C, make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas.
Embodiment 3
For a preparation method for the Nitric Acid Modified acticarbon of flue gas demercuration, specifically comprise the following steps:
1) salpeter solution that preparation molar concentration is 5mol/L, fully mixes and leaves standstill clarification;
2) being 1:1～5 according to the volume ratio of active carbon and salpeter solution, is that 20～100 object coal mass active carbons are impregnated in above-mentioned salpeter solution by the order scope of counting, and is 40 DEG C in temperature, and frequency is 40KHz, in the ultrasonic cleaning machine that power is 180W, shakes 2h; Then use distilled water repeatedly to clean after active carbon to the pH value of filtrate after modification is 7, be placed in drying box and dry 12h at 90 DEG C, make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas.
Embodiment 4
For a preparation method for the Nitric Acid Modified acticarbon of flue gas demercuration, specifically comprise the following steps:
1) salpeter solution that preparation molar concentration is 8mol/L, fully mixes and leaves standstill clarification;
2) being 1:2 according to the volume ratio of active carbon and salpeter solution, is that 20～100 object active fruit shell carbons are impregnated in above-mentioned salpeter solution by the order scope of counting, and is 60 DEG C in temperature, and frequency is 40KHz, in the ultrasonic cleaning machine that power is 220W, shakes 1h; Then use distilled water repeatedly to clean after active carbon to the pH value of filtrate after modification is 7, be placed in drying box and dry 24h at 110 DEG C, make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas.
Embodiment 5
For a preparation method for the Nitric Acid Modified acticarbon of flue gas demercuration, specifically comprise the following steps:
1) salpeter solution that preparation molar concentration is 6mol/L, fully mixes and leaves standstill clarification;
2) being 1:1 according to the volume ratio of active carbon and salpeter solution, is that 40～80 object cocoanut active charcoals are impregnated in above-mentioned salpeter solution by the order scope of counting, and is 25 DEG C in temperature, and frequency is 40KHz, in the ultrasonic cleaning machine that power is 150W, shakes 1h; Then use distilled water repeatedly to clean after active carbon to the pH value of filtrate after modification is 7, be placed in drying box and dry 20h at 80 DEG C, make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas.
Nitric Acid Modified acticarbon and original activity charcoal that the embodiment of the present invention 5 is obtained carry out activity rating:
Accurately take 50mg acticarbon, be placed in the fixed bed reactors of 120 DEG C, entrance mercury concentration is 136ug/m
3, total gas flow rate 600ml/min, the concentration of test fixed bed outlet mercury, activity rating result is as Fig. 1.
The not enough 1min of unmodified active carbon time of break-through (AC-P) as shown in Figure 1, active carbon (AC-N) after Nitric Acid Modified still has certain mercury adsorption capacity through the mercury adsorption experiment of 500min, the removal amount of mercury reaches 222ug/g, illustrates that gained Nitric Acid Modified active carbon of the present invention improves greatly with respect to the demercuration efficiency of original activity charcoal.
The present invention has utilized nitric acid can increase this characteristic of activated carbon surface functional group, and in the time that the flue gas composition that contains mercury enters the pore passage structure of active carbon, mercury be hunted down.In the present invention, Nitric Acid Modified active carbon is a kind of high-efficiency mercury removal adsorbent that is exclusively used in power station, Industrial Boiler, Industrial Stoves coal-fired flue-gas injection demercuration technology, operation and preparation process have that energy consumption is low, simple to operate, low cost and other advantages, and the ability of the charcoal absorption mercury after modification is greatly improved, can effectively control the mercury in coal-fired flue-gas.
Applicant's statement, the present invention illustrates preparation method of the present invention by above-described embodiment, but the present invention is not limited to aforesaid operations step, does not mean that the present invention must rely on aforesaid operations step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the selected raw material of the present invention and the interpolation of auxiliary element, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characterictic described in above-mentioned detailed description of the invention, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible combinations.
In addition, between various embodiment of the present invention, also can be combined, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. for a preparation method for the Nitric Acid Modified acticarbon of flue gas demercuration, it is characterized in that, said method comprising the steps of:
1) salpeter solution of preparation molar concentration >=1mol/L, mixes and leaves standstill clarification;
2) active carbon is impregnated into step 1) in described salpeter solution, ultrasonic concussion 0.5～4h; Then make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas through washing, oven dry.
2. the method for claim 1; it is characterized in that; described active carbon is the mixture of a kind of in cocoanut active charcoal, coal mass active carbon, active fruit shell carbon, bamboo granular activated carbon or Powdered Activated Carbon or at least two kinds; preferably cocoanut active charcoal and/or active fruit shell carbon, further preferred cocoanut active charcoal.
3. method as claimed in claim 1 or 2, is characterized in that step 1) molar concentration >=3mol/L of described salpeter solution, preferably 5～8mol/L, further preferred 6mol/L.
4. the method as described in one of claim 1-3, is characterized in that step 2) particle diameter of described active carbon is 20～100 orders, preferably 30～90 orders, further preferred 40～80 orders;
Preferably, the volume ratio of described active carbon and salpeter solution is 1:1～5, further preferred 1:1～1:2, most preferably 1:1.
5. the method as described in one of claim 1-4, is characterized in that, described ultrasonic temperature is 25～100 DEG C, preferably 25～60 DEG C, and further preferably 25～40 DEG C, most preferably 25 DEG C;
Preferably, described supersonic frequency is 40KHz;
Preferably, described ultrasonic power is 120～300W, preferably 120～220W, further preferably 120～180W, most preferably 150W;
Preferably, the described concussion time is 0.5～2h, further preferably 0.5～1h, most preferably 1h.
6. the method as described in one of claim 1-5, is characterized in that step 2) described washing methods is that to use distilled water active carbon to the pH value of filtrate of repeatedly cleaning after modification be 7.
7. the method as described in one of claim 1-6, is characterized in that, the described bake out temperature of step (2) is at least 60 DEG C, preferably at least 80 DEG C, and more preferably 110 DEG C;
Preferably, described drying time is at least 8h, is preferably 8～24h, more preferably 12～24h, most preferably 15h.
8. the method as described in one of claim 1-7, is characterized in that, said method comprising the steps of:
1) salpeter solution that preparation molar concentration is 6mol/L, fully mixes and leaves standstill clarification;
2) being 1:1 according to the volume ratio of active carbon and salpeter solution, is that 40～80 object active carbons are impregnated in above-mentioned salpeter solution by the order scope of counting, and is 25 DEG C in temperature, and frequency is 40KHz, and power is to shake 1h in 150W ultrasonic cleaning machine; Then wash, dry and make demercuration Nitric Acid Modified acticarbon in coal-fired flue-gas.
9. a Nitric Acid Modified acticarbon, is characterized in that, described adsorbent prepares by the method as described in one of claim 1-7.
10. a purposes for Nitric Acid Modified acticarbon as claimed in claim 9, is characterized in that, described Nitric Acid Modified acticarbon is applied in power station, Industrial Boiler, industrial furnace smoke injection demercuration technology.
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| CN106824251A (en) * | 2016-12-23 | 2017-06-13 | 吉林大学 | The combined material and catalysis treatment method of water and soil are polluted in a kind of catalytic treatment |
| CN113731356A (en) * | 2021-07-07 | 2021-12-03 | 生态环境部华南环境科学研究所 | Modified activated carbon adsorbent and preparation method and application thereof |
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| CN106732434A (en) * | 2017-01-24 | 2017-05-31 | 福州大学 | A kind of method that acticarbon is prepared based on humic acid dipping |
| CN113012943A (en) * | 2021-02-25 | 2021-06-22 | 海南大学 | Active carbon modification method for zinc ion hybrid capacitor |
| CN114588877A (en) * | 2022-02-23 | 2022-06-07 | 木林森活性炭江苏有限公司 | Modified activated carbon carrier, liquid-phase chlorosilane impurity-removing adsorbent and production process of adsorbent |
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