CN110451504A - The method that microwave heating auxiliary one step activation of vapor prepares active carbon from coal - Google Patents
The method that microwave heating auxiliary one step activation of vapor prepares active carbon from coal Download PDFInfo
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Abstract
The present invention discloses the method that microwave heating auxiliary one step activation of vapor prepares active carbon from coal, source of iron is added in coal dust and carries out microwave irradiation and be passed through vapor activating, ferro element in the mixture after activation is being removed and is being dried using hydrochloric acid.The present invention uses microwave radiation method to prepare active carbon for low-order coal and provides thermal energy, and for the intensity for increasing active carbon, a small amount of Fe base catalyst is adulterated into coal dust, adjusts the content of class graphite microcrystal；Remove Fe after pickling, form apparent central hole structure, microwave heating and steam activation is compound prepare active carbon from coal during, microwave irradiation will increase the defect of carbon structure, increase reaction active site, to promote the reaction rate of vapor and carbon structure.The increase of carbon structure defect can also promote the generation of activated carbon surface functional group, make the quantity of oxygen-containing functional group not less than 9.5mmol/g, the oxygen-containing functional group quantity of generation is individually activated much higher than vapor.
Description
Technical field
The invention belongs to technical field of active carbon, more particularly, are related to microwave heating auxiliary one step of vapor activation
The method and products thereof for preparing active carbon from coal.
Background technique
Preparing active carbon from coal mainly uses gas activation at present, a large amount of without addition compared with chemical activation method
Chemicals, not only production cost is low, and avoids equipment corrosion and environmental pollution.Gas activation is by feed coal through charcoal
After change process, priming reaction is carried out with carbonized material at a certain temperature using activated gas, ultimately forms flourishing pore structure,
And there is certain surface chemistry.Carbonization process usually carries out under 600~750 DEG C of inert atmospheres, decomposes random in coal
Then carbon and strengthen microstructure carbon, to improve the intensity of active carbon；Activation process is usually carried out at 750~950 DEG C, the work of use
Changing gas is often certain density vapor, CO2, low concentration O2Or its mixed gas etc., it is anti-by gas and the oxidation of carbon content in coal structure
It answers, ultimately generates the active carbon with abundant pore structure and surface functional group.
The charing of active carbon preparation and activation process are required to a large amount of thermal energy, conventional heating (hot fume purging etc.) condition
Under, material particles are the heating process of ecto-entad, and heating rate is lower, and heating time is long, and the easy uneven heating of material is even.
Activated gas vapor, CO2Etc. being weak oxide gas, lower with the reaction rate of carbon content in coal structure, activation time is long, and
Generate activated coke surface functional group limited amount, can not enhancement activated carbon absorption and catalytic performance.In addition, for a long time by outer
Inside activation process also will cause the serious surface of active carbon particle and burn mistake, to reduce the charcoal rate that obtain, improve preparation cost.
In contrast, the advantage that microwave heating has body formula, selectively heats, is non-contact thermal, there is heating speed
Rate is high, particles by heat is uniform, being capable of quick start and the characteristics of stop.The crystallite carbon structure and inorganic ash content being distributed in feed coal
Etc. good wave-sucking performance is all had, being conducive to microwave electromagnetic can be to the conversion of thermal energy, therefore coal activated carbon process has benefit
With the condition of microwave heating.In addition, microwave heating process can cause the defect sturcture of carbon, activated carbon surface functional group can be promoted
Generation.
Summarizing existing gas activation and preparing main problem existing for active carbon from coal is:
(1) charing, activation process need a large amount of thermal energy, when using conventional heating mode, such as heat convection (hot fume
Wash away), heat transfer (particle ecto-entad carry out heat transfer), there are the disadvantages such as rate of heat transfer is low, heating time is long, energy consumption height
End, and particles by heat unevenness is be easy to cause to reduce the performance of active carbon.
(2) carbonization process is usually carried out at 600~750 DEG C, and (it is micro- that strong polycondensation forms class graphite for the reinforcing of crystallite carbon structure
It is brilliant) usually just had obvious effects at 1000 DEG C or more, therefore it is relatively low at a temperature of can not effectively improve the strong of active carbon
Degree, especially to the lower low-order coal of crystallite carbon content, active carbon intensity usually obtained is low, easy to wear.
(3) if improving carbonization temperature to 1000 DEG C or more, class graphite microcrystalline structure increases, and reaction active site is reduced, and increases
Next step activation process vapor, CO are added2Deng the difficulty reacted with carbon structure, and then influence the generation of pore structure.Therefore,
When charing, activation are carried out in two steps, there is the contradiction between structural strength and porosity.
(4) in activation process, vapor, CO2Deng for weak oxide gas, what is generated after reacting with carbon structure is oxygen-containing
Number of functional groups is lower, is unfavorable for further increasing the absorption of active carbon and catalytic performance.
(5) existing that active carbon is prepared using microwave heating method, it is mostly rich for classes graphite microcrystalline structures such as petroleum coke, pitches
Rich raw material, and individually microwave heating can not generate a large amount of micropores and central hole structure.The chemicals such as KOH are added to produce largely
Micropore, but mesoporous is undeveloped, and a large amount of chemicals (mass ratio of KOH and coal is generally greater than 1:1) be easy to cause equipment corrode and
Environmental pollution.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of microwave heating auxiliary one step of vapor activation
The method for preparing active carbon from coal, microwave heating and steam activation is compound prepare active carbon from coal during, microwave irradiation
It will increase the defect of carbon structure, increase reaction active site, thus promote the reaction rate of vapor and carbon structure, carbon structure defect
Increase can also promote the generation of activated carbon surface functional group, vapor reacts in carbon structure active sites, mainly generates
Microcellular structure.
Technical purpose of the invention is achieved by following technical proposals:
A kind of method that the one step activation of vapor of microwave heating auxiliary prepares active carbon from coal, carries out as steps described below:
Step 1, ferro element is added to it is in coal dust and evenly dispersed, ferro element additive amount be quality of pc 3-15%；
It selects Iron(III) chloride hexahydrate or Fe(NO3)39H2O to provide ferro element, is added in coal dust mixed using ball-milling method
It closes uniformly, drum's speed of rotation is 1000rad/min~2000rad/min, and Ball-milling Time is 60min~120min；
Coal dust selects low rank coal, i.e. low-order coal, such as lignite, ub-bituminous coal (performance and lignite are close in bituminous coal).
Moreover, in step 1, ferro element additive amount is 5-the 10% of quality of pc.
Moreover, in step 1, being uniformly mixed using ball-milling method, drum's speed of rotation is 1500rad/min~1800rad/
Min, Ball-milling Time are 80min~100min.
Step 2, to the mixed powder obtained by step 1 while microwave irradiation and steam activation are carried out, to be lived
Material after change；
The mixed material obtained by step 1 is put into microwave generator, under conditions of microwave irradiation, is passed through vapor
It is activated, microwave output power is 300W~600W, provides water using the mixed gas of vapor and inert protective gas and steams
Gas, vapor percentage by volume are 30~60%, and inert protective gas percentage by volume is 40-70%, every 10g mixed material
Logical mixed gas flow be 300mL/min~500mL/min, activation time is in 30min~100min；
Moreover, in step 2, microwave output power is 350W~550W, uses the mixed of vapor and inert protective gas
It closes gas and vapor is provided, vapor percentage by volume is 35~50%, and inert protective gas percentage by volume is 50-65%,
Every 10g mixed material logical mixed gas flow be 350mL/min~450mL/min, activation time is in 40min~80min.
Moreover, in step 2, inert protective gas is nitrogen, helium or argon gas.
Step 3, material carries out acid soak and obtains active carbon to remove ferro element after the activation prepared by step 2；
Acid soak is carried out to material after activation using hydrochloric acid, concentration of hydrochloric acid is 1mol/L~2mol/L, object after every 10g activation
Hydrochloric acid dosage needed for expecting is 100mL~160mL, and soaking time is 1h~5h, then with deionized water wash products up to no chlorine
Ion detection goes out.
Moreover, in step 3, hydrochloric acid dosage needed for material is 120mL~140mL, soaking time 2h after every 10g activation
~4h, then with deionized water wash products up to no chloride test goes out.
Step 4, the active carbon handled through step 3 carries out to drying to constant weight to remove moisture removal, to obtain active carbon from coal.
The active carbon that step 3 is handled is placed in drying box in air atmosphere and dries, drying temperature be 80 DEG C~
90 DEG C, the slow oxidation of low-order coal active carbon is avoided, the active carbon from coal of structural strength height, hole prosperity is obtained after dry.
Moreover, in step 4, drying temperature is 80-85 degrees Celsius.
The present invention also provides the active carbon from coal prepared according to the above method, the class graphite microcrystal group with shortrange order is micro-
Pattern is seen, mesopore volume is not less than 0.25cm3/ g, Micropore volume are not less than 0.2cm3The quantity of/g, oxygen-containing functional group are not less than
9.5mmol/g。
Moreover, mesopore volume is average up to 0.25-0.5cm3/ g, Micropore volume are average up to 0.2-0.3cm3/ g, it is oxygen-containing
The quantity of functional group is average up to 9-13mmol/g.
Compared with prior art, technical solution of the present invention has a characteristic that
(1) it uses microwave radiation method to prepare active carbon for low-order coal and provides thermal energy-using the microcrystalline carbon of natural distributed in coal
Structure and inorganic ash content can be realized and are rapidly heated as wave absorbing agent, and heating rate can be higher than 80 DEG C/min, by controlling microwave
Power can regulate and control heating rate；The characteristics of microwave body formula, selectivity heating, so that heated simultaneously inside and outside each particle and particle,
Material is heated evenly.
(2) it is the intensity for increasing active carbon, a small amount of Fe base catalyst (i.e. ferro element) is adulterated into low-order coal, since Fe has
There is good wave-sucking performance, localized hyperthermia can be generated at 1000 DEG C or more, and Fe has the function of catalyzed graphitization, therefore
The intensity that a large amount of class graphite microcrystalline structures improve active carbon can be formed around Fe；Being rapidly heated can with catalyzed graphitization process
Prolonged carbonization process is substituted, and then realizes that a step activation prepares active carbon from coal；By controlling the content of Fe base catalyst,
The content of class graphite microcrystal can be adjusted.
(3) Fe is removed after pickling, forms apparent central hole structure, therefore Fe base catalyst not only has catalyzed graphitization
Effect, also have the function of mesoporous template；Under microwave heating use Fe base catalyst, effectively overcome degree of graphitization and
Contradiction between porosity；By adjusting the content of Fe base catalyst, central hole structure can be regulated and controled, so that mesopore volume is not less than
0.25cm3/g。
(4) microwave heating and steam activation is compound prepare active carbon from coal during, microwave irradiation will increase carbon knot
The defect of structure increases reaction active site, to promote the reaction rate of vapor and carbon structure；The increase of carbon structure defect also can
The generation for promoting activated carbon surface functional group makes the quantity of oxygen-containing functional group not less than 9.5mmol/g, independent much higher than vapor
The oxygen-containing functional group quantity (6.8mmol/g) generated is activated, by adjusting microwave irradiation intensity and time, controls oxygen-containing functional group
Quantity.
(5) microwave heating with steam activation is compound prepare active carbon from coal during, vapor carbon structure activity
It reacts on position, mainly generates microcellular structure, by adjusting water vapor concentration and activation time, Micropore volume is adjusted, makes
It obtains Micropore volume and is not less than 0.2cm3/g。
Detailed description of the invention
Fig. 1 be in the present invention Fe base catalyst (ferro element) additive amount to the influence curve of the mesopore volume of active carbon from coal
Figure.
Fig. 2 is the transmission electron microscope photo of active carbon from coal of the invention.
Fig. 3 be in the present invention activation time to the influence curve figure of the Micropore volume of active carbon from coal.
Fig. 4 is the influence curve in the present invention using different heating mode to active carbon from coal surface oxygen functional group quantity
Figure.
Specific embodiment
Technical solution of the present invention is further illustrated combined with specific embodiments below.
Using the eastern coal of standard in low-order coal (i.e. the coal of low metamorphic grade) in the embodiment of the present invention, as coal dust raw material,
It is as shown in the table:
Using Micromeritics company ASAP2020 surface area and pore structure study instrument, the hole of sample is held and is divided
Analysis: being put into de-aeration stage for test sample first, deaerates 8h, is then analyzed, with high-purity N in 473K under vacuum condition2To inhale
Attached matter measures relative pressure (P/P at liquid nitrogen temperature (77.3K)0)10-7Absorption, desorption isotherm in~1 range；By opposite
Liquid nitrogen adsorptive value calculates liquid nitrogen volume as total pore volume, using DR equation calculation Micropore volume, mesopore volume when pressure is 0.98
Micropore volume is subtracted for total pore volume.
It is tested by temperature programmed desorption (TPD), the quantity-of test activated carbon surface oxygen-containing functional group uses program liter
Warm detachment assays system mainly includes temperature programmed control tubular heater, heat tracing carrying pipe and portable fourier-transform infrared light
Spectrometer (Gasment-DX4000 type).Portable Fourier transformation infrared spectrometer can measure gas component change with on-line continuous
Change.2.0g sample is weighed, is laid in horizontal pipe furnace, heat temperature raising.Escaping gas is by high-purity N2(1L/min) is carried, warp
Conduit with heating tape is continually fed into portable Fourier transformation infrared spectrometer and measures gas concentration (CO, CO2And H2O)。
Tube furnace initial temperature is set as 110 DEG C, stops 20min drying and dehydrating, is then warming up to 1000 DEG C with 8 DEG C/min.Temperature-rise period
In, oxygen-containing functional group is thermally decomposed, with CO or CO2Form evolution.It is measured by portable Fourier transformation infrared spectrometer
CO and CO2Lasting evolution concentration, then it is integrated calculate 110 DEG C~1000 DEG C heating process be precipitated CO and CO2Total amount
Correspondence obtains the total amount of the oxygen-containing functional groups such as phenolic hydroxyl group, carboxyl, lactone group, ether, carbonyl, quinonyl, pyranone and chromene.
Embodiment 1
Use six hydration FeCl3It is added in raw coal coal dust, is uniformly mixed using ball-milling method, wherein Fe element accounts for coal dust matter
The 8% of ratio is measured, drum's speed of rotation 1500rad/min, Ball-milling Time 100min obtain coal dust intermixture.In microwave irradiation
Under conditions of, steam activation, microwave output power 450W, vapor volumetric concentration (volume hundred are carried out to coal dust intermixture
Score) it is 50%, other gases are nitrogen, and the flow that every 10g mixture institute water flowing steam and nitrogen mix gas is 400mL/min,
Activation time is 60min.Mixture after activation salt acid soak is removed into Fe element, concentration of hydrochloric acid 1mol/L, every 10g are mixed
Hydrochloric acid dosage needed for closing object is 120mL, soaking time 2h, then with deionized water wash products up to no chloride test
Out.Active carbon after washing is dried at 80 DEG C, the active carbon from coal of structural strength height, hole prosperity is obtained after dry.
Embodiment 2
Using with the consistent technological parameter of embodiment 1, adjust ferro element account for quality of pc ratio be 4%, 6% and 10%, point
The active carbon of different ferro element additive amounts is not prepared, the relationship of pore volume and ferro element additive amount in investigation.It lives to increase
Property charcoal intensity, a small amount of Fe base catalyst (i.e. ferro element) is adulterated into low-order coal, due to Fe have good wave-sucking performance, energy
Localized hyperthermia is enough generated at 1000 DEG C or more, and Fe has the function of catalyzed graphitization, therefore can be formed around Fe big
Class graphite microcrystal can be adjusted by controlling the content of Fe base catalyst by measuring the intensity that class graphite microcrystalline structure improves active carbon
Content the class graphite microcrystal group of shortrange order can be observed by Fig. 2 images of transmissive electron microscope, class graphite microcrystalline structure can be improved
The intensity of active carbon；Fe is removed after pickling simultaneously, forms apparent central hole structure, Fe base catalyst not only has catalytic graphite
The effect of change also has the function of mesoporous template, by adjusting the content of Fe base catalyst, can regulate and control central hole structure, make
It obtains mesopore volume and is not less than 0.25cm3/ g-only changes the mass ratio that Fe element accounts for coal dust, when mass ratio is increased to from 3%
10%, mesopore volume is from 0.25cm3/ g increases to 0.40cm3/g。
Embodiment 3
Using with the consistent technological parameter of embodiment 1, adjustment activation time be 40 and 80min, difference is prepared respectively
The active carbon of activation time investigates the relationship of micropore volume and activation time.Microwave heating with steam activation is compound prepares coal
During matrix activated carbon, vapor reacts in carbon structure active sites, mainly generates microcellular structure, is steamed by adjusting water
Micropore volume is adjusted in gas concentration and activation time, so that Micropore volume is not less than 0.2cm3/ g-only changes steam activation
Time, when activated between from 40min increase to 80min, Micropore volume is from 0.21cm3/ g increases to 0.27cm3/g。
Embodiment 4
Using with the consistent technological parameter of embodiment 1, use electric furnace instead and heated, i.e., ball-milling method after mixing, in electricity
The mixed gas of vapor and nitrogen is passed through in the environment of stove heating, control electric furnace heating temperature is 800-850 degrees Celsius, than
Compared with the oxygen-containing functional group quantity of the two.Microwave heating and steam activation is compound prepare active carbon from coal during, microwave spoke
Note increases the defect of carbon structure, increases reaction active site, to promote the reaction rate of vapor and carbon structure；Carbon structure lacks
Sunken increase can also promote the generation of activated carbon surface functional group, make the quantity of oxygen-containing functional group not less than 9.5mmol/g, remote high
The oxygen-containing official of (i.e. only steam activation, electric furnace heating do not cause corresponding activation effect) generation is individually activated in vapor
Quantity (6.8mmol/g) can be rolled into a ball.
Embodiment 5
It is added in raw coal coal dust using Fe(NO3)39H2O, is uniformly mixed using ball-milling method, wherein Fe element accounts for coal dust
The 10% of mass ratio, drum's speed of rotation 1800rad/min, Ball-milling Time 120min obtain coal dust intermixture.In microwave spoke
According under conditions of, steam activation, microwave output power 500W, vapor volumetric concentration (volume are carried out to coal dust intermixture
Percentage) it is 60%, other gases are nitrogen, and the flow that every 10g mixture institute water flowing steam and nitrogen mix gas is 500mL/
Min, activation time 80min.By the mixture after activation with salt acid soak remove Fe element, concentration of hydrochloric acid 2mol/L, often
Hydrochloric acid dosage needed for 10g mixture is 120mL, soaking time 2h, then with deionized water wash products up to no chloride ion
It detects.Active carbon after washing is dried at 80 DEG C, it is high, hole prosperity coal based activated that structural strength is obtained after dry
Charcoal.
Content is adjusted technological parameter according to the present invention, and microwave heating auxiliary one step of vapor activation system can be achieved
The technical solution of standby active carbon from coal, and product shows the performance almost the same with embodiment.The present invention is shown above
Example property description, it should explanation, in the case where not departing from core of the invention, it is any it is simple deformation, modification or
Other skilled in the art can not spend the equivalent replacement of creative work to each fall within protection scope of the present invention.
Claims (10)
1. the method that microwave heating auxiliary one step activation of vapor prepares active carbon from coal, which is characterized in that as steps described below
It carries out:
Step 1, ferro element is added to it is in coal dust and evenly dispersed, ferro element additive amount be quality of pc 3-15%, selection
Iron(III) chloride hexahydrate or Fe(NO3)39H2O provide ferro element, and coal dust selects low rank coal；
Step 2, to the mixed powder obtained by step 1 while microwave irradiation and steam activation are carried out, after obtaining activation
Material；The mixed material obtained by step 1 is put into microwave generator, under conditions of microwave irradiation, be passed through vapor into
Row activation, microwave output power are 300W~600W, provide vapor using the mixed gas of vapor and inert protective gas,
Vapor percentage by volume is 30~60%, and inert protective gas percentage by volume is 40-70%, and every 10g mixed material leads to
The flow of mixed gas is 300mL/min~500mL/min, and activation time is in 30min~100min；
Step 3, material carries out acid soak and obtains active carbon to remove ferro element after the activation prepared by step 2；
Step 4, the active carbon handled through step 3 is dried, to obtain active carbon from coal.
2. the method that microwave heating auxiliary one step activation of vapor according to claim 1 prepares active carbon from coal, special
Sign is, in step 1, selects Iron(III) chloride hexahydrate or Fe(NO3)39H2O to provide ferro element, is added in coal dust and adopts
With ball-milling method be uniformly mixed, drum's speed of rotation be 1000rad/min~2000rad/min, Ball-milling Time be 60min~
120min；Coal dust is lignite or ub-bituminous coal.
3. the method that microwave heating auxiliary one step activation of vapor according to claim 1 prepares active carbon from coal, special
Sign is that in step 1, ferro element additive amount is 5-the 10% of quality of pc, is uniformly mixed using ball-milling method, and ball mill turns
Speed is 1500rad/min~1800rad/min, and Ball-milling Time is 80min~100min.
4. the method that microwave heating auxiliary one step activation of vapor according to claim 1 prepares active carbon from coal, special
Sign is that in step 2, microwave output power is 350W~550W, uses the mixed gas of vapor and inert protective gas
Vapor is provided, vapor percentage by volume is 35~50%, and inert protective gas percentage by volume is 50-65%, every 10g
Mixed material logical mixed gas flow be 350mL/min~450mL/min, activation time is in 40min~80min；In step
In rapid 2, inert protective gas is nitrogen, helium or argon gas.
5. the method that microwave heating auxiliary one step activation of vapor according to claim 1 prepares active carbon from coal, special
Sign is, in step 3, carries out acid soak to material after activation using hydrochloric acid, concentration of hydrochloric acid is 1mol/L~2mol/L, often
Hydrochloric acid dosage needed for material is 100mL~160mL after 10g activation, and soaking time is 1h~5h, then cleans production with deionized water
Object goes out up to no chloride test；It is preferred that hydrochloric acid dosage needed for material is 120mL~140mL after every 10g activation, soaking time is
2h~4h.
6. the method that microwave heating auxiliary one step activation of vapor according to claim 1 prepares active carbon from coal, special
Sign is that in step 4, the active carbon that step 3 is handled is placed in drying box in air atmosphere and dries, drying temperature
For 80 DEG C~90 DEG C, preferably 80-85 degrees Celsius, avoid low-order coal active carbon from slowly aoxidizing, after dry.
7. the method that microwave heating auxiliary one step activation of vapor according to claim 1 prepares active carbon from coal, special
Sign is, by adjusting the content of Fe base catalyst (i.e. ferro element), regulates and controls central hole structure, the class graphite microcrystal of active carbon from coal
Content.
8. the method that microwave heating auxiliary one step activation of vapor according to claim 1 prepares active carbon from coal, special
Sign is, by adjusting microwave irradiation intensity and time, controls the oxygen-containing functional group quantity of active carbon from coal；It is steamed by adjusting water
Gas concentration and activation time adjust the Micropore volume of active carbon from coal.
9. active carbon from coal prepared by the method as described in one of claim 1-8, which is characterized in that active carbon from coal has
Class graphite microcrystal group's microscopic appearance of shortrange order, mesopore volume are not less than 0.25cm3/ g, Micropore volume are not less than 0.2cm3/ g,
The quantity of oxygen-containing functional group is not less than 9.5mmol/g.
10. active carbon from coal according to claim 9, which is characterized in that mesopore volume is average up to 0.25-0.5cm3/
G, Micropore volume are average up to 0.2-0.3cm3/ g, the quantity of oxygen-containing functional group are average up to 9-13mmol/g.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113332954A (en) * | 2021-04-14 | 2021-09-03 | 武汉科技大学 | Sintered flue gas denitration adsorbent and preparation method and application thereof |
| CN114377653A (en) * | 2021-12-17 | 2022-04-22 | 农业部沼气科学研究所 | Directional rapid modification method of oxygen-containing functional groups on surface of activated carbon |
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2018
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113332954A (en) * | 2021-04-14 | 2021-09-03 | 武汉科技大学 | Sintered flue gas denitration adsorbent and preparation method and application thereof |
| CN113332954B (en) * | 2021-04-14 | 2022-06-07 | 武汉科技大学 | Sintered flue gas denitration adsorbent and preparation method and application thereof |
| CN114377653A (en) * | 2021-12-17 | 2022-04-22 | 农业部沼气科学研究所 | Directional rapid modification method of oxygen-containing functional groups on surface of activated carbon |
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