CN105905898A - Preparation method of coal-based agglomerated activated carbon with high methylene blue value - Google Patents
Preparation method of coal-based agglomerated activated carbon with high methylene blue value Download PDFInfo
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Abstract
The invention discloses a preparation method of a coal-based agglomerated activated carbon with high methylene blue value. The method includes: taking long flame coal, gas-fat coal and asphalt as the raw materials to conduct coal blending, and conducting mixing with zinc chloride, and performing crushing to obtain feed coal; carrying out briquetting and granulation on the feed coal to obtain coal particles; performing oxidation treatment and carbonization treatment on the coal particles to obtain a carbonized material; using a zinc chloride solution to immerse the carbonized material, performing solid-liquid separation and drying, and subjecting the obtained immersed carbonized material to activation treatment so as to obtain activated carbon. The method provided by the invention utilizes a certain amount of long flame coal, gas-fat coal and asphalt to prepare activated carbon, well combines the properties of the raw materials and the cooperation between each other, compared with traditional coal-based agglomerated activated carbon, under the action of a zinc chloride compound additive, the methylene blue value of the activated carbon product can be effectively enhanced, and the problem of poor methylene blue adsorption ubiquitous in traditional coal-based agglomerated activated carbon production can be solved.
Description
Technical field
The invention belongs to activated carbon preparation field, particularly to the coal base briquetting of a kind of high methylene blue number
The preparation method of activated carbon.
Background technology
Owing to activated carbon has highly developed pore structure and great specific surface area, it applies model
Enclose from decolouring and taste removal, the canister respirator for food and medicine, develop into extensive for solvent
Refine and recovery, water depth process, gas cleaning, blood purification etc., the adsorptivity to activated carbon
New, higher requirement can be proposed.
Activated carbon can be divided into active carbon from coal, petroleum coke activated carbon, wooden activity according to raw material difference
Charcoal and active fruit shell carbon etc., wherein, petroleum coke activated carbon, wood activated charcoal and active fruit shell carbon etc.
Owing to raw material sources are the most limited, it is difficult to long-term large-scale production, simultaneously as Chinese coal money
Source is enriched, and yield is big, and from the horse's mouth, the yield of active carbon from coal increases year by year, and it utilizes
Scope is more and more wider.Dividing according to form, activated carbon includes pressed active carbon and powdered activated carbon,
Wherein powdered activated carbon possesses bigger adsorptivity (iodine number and/or methylene blue compared to pressed active carbon
Value), but due to its powder form, limit application.
Based on above reason, the production of coal base agglomerated activated carbon increasingly comes into one's own.Along with society
Development, water pollutant component is the most complicated, and macromole chemical industry organic pollution is gradually increased.This
Just require that activated carbon product, on the basis of absorption tradition pollutant, is also wanted to adsorb the organic dirt of chemical industry
Dye thing.The active carbon from coal micropore that common process produces is flourishing, very strong to tradition pollutant adsorptivity,
But absorption macromole chemical industry organic pollution or the mesopore that needs as charcoal carrier are then and undeveloped,
Show as methylene blue number on the low side, it is impossible to full macromole chemical industry pollutant and charcoal carrier media, and
Traditional promote methylene blue and be worth method by increasing soak time, reduce yield iodine sorption value and
Intensity.
CN1248962C discloses the preparation method of a kind of agglomerated activated carbon, wherein, will by weakly caking coal,
The raw material of coking coal and coal tar pitch composition mixes with alkali metal hydroxide, pulverizes, after briquetting pelletize,
Activated carbon is made through carbonization and activation, but, first and last, the methylene blue number of its activated carbon product
The most on the low side with iodine number, but also need to use highly basic, big to environment hidden danger.
Summary of the invention
It is an object of the invention to provide the preparation side of the coal base agglomerated activated carbon of a kind of high methylene blue number
Method, to solve the problem that during traditional coal base agglomerated activated carbon produces, methylene blue adsorptivity is poor.
For achieving the above object, the present invention is by the following technical solutions:
The preparation method of the coal base agglomerated activated carbon of a kind of high methylene blue number, comprises the steps:
A, utilize jet coal, gas rich coal and Colophonium for raw material carry out coal blending and mix with zinc chloride, powder
Broken to obtain feed coal, wherein, in terms of the gross weight of described feed coal, the consumption of described jet coal
For 65wt%-80wt%, the consumption of gas rich coal is 15wt%-25wt%, and the consumption of Colophonium is
3wt%-7wt%, the consumption of zinc chloride is 2wt-5wt%；
B, by described feed coal compound stalk forming, pelletize, obtain coal particle；
C, described coal particle is carried out oxidation processes, carbonization process, obtain carbonized material；
D, utilize liquor zinci chloridi impregnate described carbonized material, solid-liquid separation post-drying, the leaching that will obtain
Stain carbonized material carries out activation processing, with prepared activated carbon.
In the preparation process in accordance with the present invention, step a is former for utilizing jet coal, gas rich coal and Colophonium
Material carries out coal blending and mixes with zinc chloride, pulverizes to obtain feed coal, concrete coal blending and crushing process
Known in the art, a certain amount of jet coal, gas rich coal, Colophonium and zinc chloride mixing can be made
Uniformly and be crushed to less particle size, 170 mesh, 180 mesh or 200 mesh sieve (Taylors are such as crossed
Standard screen).Research finds, when using above-mentioned raw materials and with aforementioned proportion coal blending, is conducive to promoting
The methylene blue number of last obtained agglomerated activated carbon, it is preferable that jet coal in described feed coal
Consumption is 70wt%-75wt%, such as 72wt%, and the consumption of gas rich coal is 15wt%-20wt%, than
Such as 18wt%.
Described jet coal is young coal, used for this invention, as realizing activated carbon key property
Basic material, research finds, with the gas rich coal of the present invention with the use of time, described jet coal
Introduce the generation being conducive to activated carbon product hole, it is simple to follow-up reaming, thus promote activated carbon
The methylene blue number of product.Preferably, the volatile matter of described jet coal is not less than 37%, such as 40%,
Light transmittance is not less than 50, such as 55, and vitrinite's content is not less than 70%, preferably not less than 75%,
Such as 80% or 85% etc., to improve the pore structure of activated carbon further；Such as, described long flame
Coal can be selected from Black Hills, Toksun coal or Qitai Beishan Mountain raw coal.
Long bituminous coal is the youngest, and internal degree of coalification is low, activity easy reaming high, follow-up.But
Owing to its degree of coalification is low, intensity is relatively low, and does not has caking property, and in carbonization process, intensity can be entered
One step reduces, and therefore at conventional carbon production field, few people produce with long bituminous coal.
Described gas rich coal is the coal of strong cohesive property, adds gas rich coal and is possible not only in the course of processing utilize
Its caking property, promotes the caking ability between pulverized coal particle, joins at the jet coal with the present invention meanwhile
When closing use, the introducing of described gas rich coal also helps formation and the strength enhancing of follow-up charcoal skeleton,
And owing to can be susceptible to shrink in follow-up carbonization process, the introducing of described gas rich coal also helps
Cause due to hypersystole being unfavorable for that the formation of Initial Crack affects subsequent activation reaming in preventing
Carrying out.Preferably, the caking index of described gas rich coal is not less than 85, for example, 90 or 95 etc.,
Cuticle thickness is not less than 25, for example, 27 or 30 etc., thus the bonding between pulverized coal particle
The absorption property promoting activated carbon product is also helped while intensity；Such as, described gas rich coal can
With selected from the suitable logical coal of Qitai Red Hill low-lying area coal or Citroen zx.
In the present invention, add Colophonium and then can guarantee that, in briquetting workshop section, there is certain initial strength,
The most described Colophonium can be that coal tar asphalt, asphalt, DCL/Direct coal liquefaction Colophonium or high temperature change
Matter coal tar pitch etc.；Preferably, described asphalt softening point > 105 DEG C, more preferably high temperature modification coal drip
Blue or green.In the present invention, the raw coal that will prepare adds the Zinc chloride solid of 2-5wt%, due to chlorination
Zinc has the effect of stronger dehydroxylation and dehydration, and at a certain temperature, the zinc chloride of addition is permissible
Make the hydrogen in raw material and oxygen release with the form of water, and be conducive to making empty reaction from inside.
In a preferred embodiment of the present invention, pulverize feed coal to obtain that there is spy
Determining the coal dust of particle size distribution, wherein, the mean diameter of the feed coal after pulverizing is not less than 20 μm, its
In, particle diameter is not more than the coal dust content of 80 μm not less than 90wt%；Particle diameter is 40 μm-80 μm
Coal dust content is not less than 10wt%.Research finds, when described coal dust has the distribution of above-mentioned dynamics,
The rational gradation composition of different-grain diameter coal dust can be realized, it is ensured that while shaping strength in forming process
There is good initial void distribution.Preferably, in described feed coal, particle diameter is not more than 80 μm
Coal dust content is not less than 95wt%；Particle diameter is not more than the coal dust content of 40 μm not less than 70wt%；
It is further preferred that the mean diameter of described coal dust is 20 μm-40 μm, such as 30 μm；More preferably
Ground, the particle diameter of described coal dust is not more than 200 μm, the most no more than 150 μm, or no more than 100 μm.
It will be appreciated by those skilled in the art that and by selecting corresponding standard screen, the feed coal after pulverizing can be entered
Row screening, thus obtain the coal dust with above-mentioned particle size distribution.
If it should be noted that above-mentioned anthracite and/or long flame pit ash exceed standard so that final
When the ash of activated carbon product is undesirable, it is right that those skilled in the art are readily apparent that before coal blending
Above-mentioned anthracite and/or long flame pit ash are controlled, such as, processed by washing deliming etc. and make institute
Stating smokeless ash and be less than 3%, the most concrete controlling extent can with the ash of final activated carbon product
It is as the criterion to meet the requirements, e.g., less than 10%.This point is known in the art, the most superfluous
State.
In the present invention, step b is for carry out compound stalk forming, pelletize to above-mentioned raw materials coal, to obtain
Coal particle.In the preparation of coal base agglomerated activated carbon, coal dust is shaped and crushes pelletize
It is processed as the conventional process of this area, such as, utilizes and roll-in block forming machine is carried out pulverized coal forming,
Crushing for example with disintegrating machine, then screening obtains the coal particle of certain particle size range, its tool
Body process is known in the art, in one embodiment, and the compound stalk forming pressure of described feed coal
Power is 10-15t/cm；Described pelletize includes broken and screening, to obtain particle diameter at 1mm-10mm,
Coal particle between more preferably 3mm-8mm.Preferably, in step b, compound stalk forming gained
The heap anharmonic ratio of briquetting coal is 660g/L-720g/L, and such as 670 or 700g/L can be become by control
Type pressure, temperature or by the way of returning charge molding, preferably control the heap anharmonic ratio of briquetting coal, Qi Zhongsuo
State returning charge molding mode be by partial briquetting molding after briquetting coal be broken for particle diameter and be not more than 3mm,
It is preferably the coal particle of 0.5-2.5mm, such as 1mm or 2mm, and described raw material ature of coal will be accounted for
The coal particle of amount 10wt%-30wt%, preferably 15wt%-25wt% returns and mixes all with described feed coal
Even, for compound stalk forming.Research finds, above-mentioned coal particle is used for walking after mixing with feed coal
Suddenly, during the compound stalk forming in b, briquetting process can preferably become the core of briquetting coal skeleton,
Thus on the basis of ensureing briquetting coal intensity, be conducive to the optimization of activated carbon internal particle further
Collection is joined, and keeps abundant space, the beneficially entrance of subsequent activation agent.
In the present invention, step c, for described coal particle carries out oxidation processes, carbonization process, obtains
To carbonized material；Pelletize gained coal particle is carried out oxidation processes, carbonization is processed as activated carbon and prepared
Conventional process step in journey, is well known to those skilled in the art.In the present invention, described oxygen
The condition that change processes can be: at 200 DEG C-250 DEG C, such as, at 220-250 DEG C, enters material
Row oxidation processes 3-6 hour, in oxidizing atmosphere, oxygen content is 6-12vol%, such as with nitrogen with empty
The gaseous mixture of gas forms oxidizing atmosphere as oxidant, so that the oxidation control of material is in lighter journey
Degree, makes part oxygen be incorporated in coal, accelerates priming reaction speed.
The condition that described carbonization processes can be: temperature 600-650 DEG C, Carbonization Atmospheres oxygen content are little
In 5vol%, carbonization processes time 15min-40min, such as 20min or 30min, after carbonization,
Charcoal atom combination in carbon compound can form the carbon structure in some cracks, has certain suction
Attached ability, these cracks will form more flourishing microcellular structure in activation procedure；Preferably,
During carbonization, material is warming up to 600 DEG C from 250 DEG C with 8-10 DEG C/min heating rate.Relatively conventional
Carbonization reaction, the present invention preferably combines the feature of feed coal, is rapidly heated and carbonization, more favorably
In subsequent activation pore-creating, and it is internal to facilitate immersion solvent to enter.
In the present invention, step d is for utilizing liquor zinci chloridi to impregnate described carbonized material, solid-liquid separation
Post-drying, carries out activation processing by the impregnated carbon material obtained, with prepared activated carbon.Impregnating
Cheng Zhong, liquor zinci chloridi can well into/penetrate in the crack of carbon structure and/or microcellular structure,
Activated positions to the zinc chloride in feed coal is formed supplementary further, and its effect is solid phase mixing institute
It is difficult to, in order to follow-up abundant activation.Preferably, the concentration of described liquor zinci chloridi is
10wt%-20wt%, dip time is 1-2h.Carbonized material after dipping is through solid-liquid separation, wherein,
Remaining liquor zinci chloridi can also impregnate next group carbonized material, and utilization ratio is high.Charcoal after separation
Material drying, the water content to carbonized material is not more than 8wt%, and such as 3wt% or 5wt% is (permissible
For activation process), obtain impregnated carbon material.In the present invention, dipping zinc chloride can be uniform
Being attached on the inwall of crack or micropore, therefore without excess, the most very few being also unfavorable for fully lives
Change.
It is the conventional process step in process for preparing active carbon that carbonized material carries out activation processing, for this
Known to skilled person.In the present invention, the condition of described activation processing is preferably: with water
Steam as activated media, at 700 DEG C-850 DEG C, such as 800 DEG C or 840 DEG C, activate
Reaction, the response time is 5-7 hour, such as 5.5 or 6.5 hours；Preferably, carbonization will be impregnated
Material is with no more than 20 DEG C/min, and the programming rate of such as 10-15 DEG C/min is warming up to 700 DEG C-800 DEG C
After, start to be passed through steam and activate, continue to heat up, and carry out stable activation at 800-850 DEG C
5.5-6 hour.Relatively conventional active carbon from coal activates, and the present invention preferably combines the feature of feed coal,
Suitably reduce activation temperature, improve activation effect, increase absorbability, prevent surface simultaneously
Overactivity.
Compared with prior art, the preparation method of the present invention has the advantage that
1, the present invention utilizes a certain amount of jet coal, gas rich coal and Colophonium coal blending to prepare activated carbon, very
Combine well character and the mating reaction each other of above-mentioned raw materials, with traditional coal base pressure
Block activated carbon is compared, and under the effect of zinc chloride compound additive, can effectively promote activated carbon
The methylene blue number of product, solves during traditional coal base agglomerated activated carbon produces the methylene blue generally existed
The problem that adsorptivity is poor；Coal base agglomerated activated carbon produced according to the invention, iodine number > 1000mg/g
Time, it is ensured that while not reducing intensity and yield, ensure that adsorptive value methylene blue number is more than 220mg/g.
2, the present invention is mixed by raw material solid phase respectively and carbonized material dipping matches and introduces in material
Zinc chloride, to improve activation effect, particularly methylene blue adsorptive value；It addition, the present invention is without making
With strongly alkaline compound, beneficially environmental protection.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail, but the present invention is not limited to this.
The characterizing method of the relevant parameter of activated carbon is described as follows:
Iodine sorption value-be measured according to GB/T7702.3-2008；
Methylene blue adsorptive value-be measured according to GB/T7702.6-2008；
Intensity-be measured according to GB/T7072.3-2008.
Remaining parameter all uses GB or this area conventional characterization mode to characterize.
In following example/comparative example, chemical reagent used is analytical pure；
Example 1
Described jet coal is colliery, Black Hills, Urumchi raw coal, and gas rich coal is Xinjiang quasi-Dong Hongshanwa gas
Rich coal.
Described Colophonium is the High softening-point modified pitch that Handan, Hebei treasured profit chemical industry is produced, and its softening point is
113-118℃。
In feed coal, jet coal content is 75wt%, gas rich coal content is 17wt%, bitumen content
It is 3wt% for 5wt%, zinc chloride content.Being pulverized by feed coal, being sized to mean diameter is 29 μm
Coal dust, wherein, particle diameter is 2.5wt% more than the coal dust content of 80 μm；Particle diameter is more than 40 μm
Coal dust content be 28wt%.
Utilizing briquetting forming machine that feed coal is carried out compound stalk forming, briquetting pressure is about 13t/cm,
The coal particle that particle diameter is 1mm-3mm that will be about feed coal weight 30% by returning material mode returns
Back pressure block, the bank proportion 690g/l suppressed, intensity 92.8.
The briquetting material obtained sieves after primary breakup and secondary breakup, and qualified pellet is carried out successively
Oxidation processes and carbonization process activation processing, and wherein oxidation processes condition is: at electrical heating external-heat
Using the tail gas mixed gas after the air and combustion of natural gas of oxygen content 11% as oxidant in converter
At 230-250 DEG C, pellet is carried out for time 3h oxidation processes；Carbonization treatment conditions are: at electricity
Material is warming up to 650 DEG C from 250 DEG C with 8-10 DEG C/min heating rate by heating external-heat converter,
Insulation 15min carries out carbonization process, and in furnace atmosphere, oxygen concentration controls less than 5vol%.
After the carbonized material obtained impregnates 80min with 15% solder(ing)acid, solid-liquid separation, drying
(wherein water content is about 4wt%, is then fed in activation furnace activation, and activation processing condition is: with
After the steam programming rate as activated media, with 10-15 DEG C/min is warming up to 700 DEG C, start
It is passed through steam to activate, continues to heat up, at 815 DEG C-825 DEG C, activate 7 hours, obtain
Activated carbon product.The indices of the activated carbon made is as follows: product iodine number 1087, intensity 97.11,
Bulk density 442, methylene blue number 272.
Embodiment 2
It is with the difference of embodiment 1: described jet coal is Qitai Beishan Mountain raw coal, gas rich coal
For Citroen zx along logical colliery producing coal.In feed coal, jet coal content is 70wt%, gas rich coal content is
20%, bitumen content be 5%, zinc chloride content be 5%.The bank proportion 670g/l suppressed,
Intensity 93.3.
Carbonization treatment conditions are: with 530-550 DEG C, material is carried out 3h in electrical heating external-heat converter
Carbonization processes.Activation processing condition is: at activated media, i.e. flow velocity be 1.5 kilogram of steam/kilogram
In the presence of the flowing steam of carbonization granule, the carbonization granule in converter is made to activate 4.5 at 889-900 DEG C
Hour, obtain activated carbon product.The indices of the activated carbon made is as follows: product iodine number 1091,
Intensity 96.87, bulk density 457, methylene blue number 252.
Embodiment 3
Being with the difference of embodiment 1: before briquetting, the feed coal after pulverizing is sized to averagely
Particle diameter is the coal dust of 22 μm, and wherein, particle diameter is 2wt% more than the coal dust content of 80 μm；Particle diameter
It is 15wt% more than the coal dust content of 40 μm.The bank proportion 700g/l suppressed, intensity 93.1.
The indices of the activated carbon made is as follows: product iodine number 1096, intensity 96.32, bulk density
439, methylene blue number 276.
Embodiment 4
It is with the difference of embodiment 1: after the feed coal after pulverizing crosses 180 mesh sieves, as
Feed coal sends into compound stalk forming in cuber.
The indices of the activated carbon made is as follows: product iodine number 1082, intensity 96.11, heap ratio
Weigh 447, methylene blue number 249.
Comparative example 1
Being with the difference of embodiment 1, in feed coal, the content of zinc chloride is 8wt%, and carbonization
Material no longer impregnates liquor zinci chloridi.
The indices of the activated carbon made is as follows: product iodine number 1079, intensity 96.7, bulk density
422, methylene blue number 223.
Comparative example 2
Being with the difference of embodiment 2, feed coal, without zinc chloride, utilizes the chlorine of 40wt%
Change zinc solution impregnated carbon material 3 hours.
The indices of the activated carbon made is as follows: product iodine number 1084, intensity 97.8, heap ratio
Weigh 452, methylene blue number 214.
Comparative example 3
Difference with embodiment 1 is, replaces with the jet coal in feed coal from Hami Poly
The weakly caking coal in colliery, replaces with the coking coal from Dahuangshan Coal Mine by gas rich coal.
The indices of the activated carbon made is as follows: product iodine number 1065, intensity 97.6, bulk density
475, methylene blue number 246.
Claims (10)
1. a preparation method for the coal base agglomerated activated carbon of high methylene blue number, comprises the steps:
A, utilize jet coal, gas rich coal and Colophonium for raw material carry out coal blending and mix with zinc chloride, powder
Broken to obtain feed coal, wherein, in terms of the gross weight of described feed coal, the consumption of described jet coal
For 65wt%-80wt%, the consumption of gas rich coal is 15wt%-25wt%, and the consumption of Colophonium is
3wt%-7wt%, the consumption of zinc chloride is 2wt-5wt%；
B, by described feed coal compound stalk forming, pelletize, obtain coal particle；
C, described coal particle is carried out oxidation processes, carbonization process, obtain carbonized material；
D, utilize liquor zinci chloridi impregnate described carbonized material, solid-liquid separation post-drying, the leaching that will obtain
Stain carbonized material carries out activation processing, with prepared activated carbon.
Preparation method the most according to claim 1, it is characterised in that in step d, described
The concentration of liquor zinci chloridi is 10wt%-20wt%, and dip time is 1-2h.
Preparation method the most according to claim 1 and 2, it is characterised in that in step a,
The mean diameter of the feed coal after pulverizing is not less than 20 μm, and wherein, particle diameter is not more than the coal of 80 μm
Powder content is not less than 90wt%；Particle diameter is that the coal dust content of 40 μm-80 μm is not less than 10wt%.
Preparation method the most according to claim 3, it is characterised in that the coal of step a gained
In powder, particle diameter is not more than the coal dust content of 80 μm not less than 95wt%；Particle diameter is not more than 40 μm
Coal dust content is not less than 70wt%.
5. according to the preparation method according to any one of claim 1-4, it is characterised in that step
In b, the heap anharmonic ratio of the briquetting coal of compound stalk forming gained is 660g/L-720g/L.
6. according to the preparation method according to any one of claim 1-5, it is characterised in that described
The volatile matter of jet coal is not less than 37%, and light transmittance is not less than 50, and vitrinite's content is not less than 70%,
It is preferably not less than 75%；The caking index of described gas rich coal is not less than 85, and cuticle thickness is not less than
25；Described Colophonium is selected from coal tar asphalt, asphalt, DCL/Direct coal liquefaction Colophonium and high temperature modification
One or more in coal tar pitch, softening point > 105 DEG C, it is preferable that described Colophonium is high temperature modification
Coal tar pitch.
7. according to the preparation method according to any one of claim 1-6, it is characterised in that described
In feed coal, the consumption of jet coal is 70wt%-75wt%, and the consumption of gas rich coal is 15wt%-20wt%.
8. according to the preparation method according to any one of claim 1-7, it is characterised in that step
In c, oxidation processes condition is: at 200 DEG C-250 DEG C, material is carried out oxidation processes 3-6 hour,
In oxidizing atmosphere, oxygen content is 6-12%.
9. according to the preparation method according to any one of claim 1-8, it is characterised in that step
In c, carbonization treatment conditions are: temperature 600-650 DEG C, Carbonization Atmospheres oxygen content are not more than 5vol%,
Carbonization processes time 20min-40min.
10. according to the preparation method according to any one of claim 1-9, it is characterised in that step
In d, activation processing condition is: using steam as activated media, carry out at 800 DEG C-850 DEG C
Priming reaction, soak time is 5-7 hour.
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Cited By (3)
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| CN109179404A (en) * | 2018-09-12 | 2019-01-11 | 宁夏宝塔石化煤化工研究院有限公司 | A method of using jet coal prepare in big mesoporous activated carbon |
| CN113019321A (en) * | 2021-03-04 | 2021-06-25 | 太原理工大学 | Coal-based particles, preparation method thereof and application thereof in filtering coal wastewater |
| CN116477622A (en) * | 2023-04-12 | 2023-07-25 | 国家能源集团新疆能源有限责任公司 | Coal-based activated carbon, preparation method and application thereof |
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