CN109399632A - A method of preparing asphalt-base globular active carbon - Google Patents
A method of preparing asphalt-base globular active carbon Download PDFInfo
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- CN109399632A CN109399632A CN201811145098.4A CN201811145098A CN109399632A CN 109399632 A CN109399632 A CN 109399632A CN 201811145098 A CN201811145098 A CN 201811145098A CN 109399632 A CN109399632 A CN 109399632A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
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Abstract
A kind of method preparing asphalt-base globular active carbon is that middle soft pitch raw material and modifying agent are added in reaction kettle; under nitrogen protection; it is stirred after being heated to 100~300 DEG C; 0.5~4 h of constant temperature, is subsequently vacuumed out, cooling discharge; obtain the modified pitch that can be used for balling-up; bitumen ball is made using emulsification pelletizing method, the bitumen ball is then placed directly within the hollow air-blowing of oxidation furnace without any processing and is swept, with 30~60 DEG C of h‑1Heating rate be warming up to 250~350 DEG C, 0.5~4 h of constant temperature is to get stabilized bitumen ball, and then by its charing-activation, i.e. acquisition asphalt-base globular active carbon.Product of the present invention sphericity is good, and intensity is higher, and can scale, the advantages of consecutive production.
Description
Technical field
The invention belongs to the preparation fields of asphalt-base globular active carbon, and in particular to it is a kind of using middle soft pitch as raw material,
The method that naphthalene prepares asphalt-base globular active carbon is not added.
Background technique
Asphalt-base globular active carbon is because its raw material sources is abundant, inexpensive, product high mechanical strength, and sphericity is high, and wide spectrum is inhaled
Attached performance is good, and adsorption desorption speed is fast, obtains in fields such as blood purification, catalyst carrier, organic solvent recycling, noble metal recycling
To popularization and application.But its preparation process and equipment are more complex, however it remains some technical problems.Currently, preparing asphalt-base globular
The basic procedure of active carbon: modulation pitch → balling-up → (pre-) oxidation → charing → activation.Currently, most and asphaltic base ball
It is to use high softening point bitumen (softening point is greater than 200 DEG C) for raw material that shaped activated carbon, which prepares relevant patent all, such as patent
CN101259961 A " a kind of preparation method of nitrogen-containing asphalt-base spherical activated "；CN101792678 A be " a kind of bitumen ball
Preparation method "；Raw material described in CN1188136 A " a method of prepare narrow size distribution asphalt ball " uses bar none
High softening point bitumen.1607174 A of patent CN " method for preparing spherical activated carbon " uses oxidizing gas or use first
Nitric acid is crosslinked and is concentrated heavy-hydrocarbon oil at 200~400 DEG C, to obtain initial elevated temperature pitch, and then prepares spherical activated carbon.So
And there are low (generally less than 60%) of yield and serious environmental pollutions in its preparation process for hard pitch, and as drip
There is also at high cost, dissolubility is poor, plastic deformation ability is insufficient, is difficult to directly soften balling-up etc. for the raw material of green base spheric active carbon
Problem.
The method of asphalt spheroidization is divided into emulsion process, spray granulation and suspension method again.Most widely used method is outstanding
Float glass process balling-up, according to " the Process for preparing spherical carbon material of patent US 4371454
And spherical activated carbon " is described, typical suspension method balling-up are as follows: by high softening point bitumen and additive
(or viscosity reductant, mainly naphthalene) melt blending forms solution altogether, then emulsifies its particle in the hot water containing dispersing agent
Then balling-up removes additive again to get bitumen ball.Other patents CN104084195 A " urge by a kind of support type spherical activated charcoal
Agent and preparation method thereof "；106348290 A of CN " a kind of preparation method of high-termal conductivity asphalt-base globular active carbon "；CN
1607174 A " method for preparing spherical activated carbon " are similar therewith.103695019 A of patent CN " one-step method low energy consumption preparation drip
The technology of green ball " report, is directly added into balling-up in normal-pressure reaction kettle for high softening point bitumen, naphthalene, dispersing agent and water, without cooling
It can be directly separated by solid-liquid separation, up to bitumen ball after solvent removing naphthalene.It can be seen that no matter for multistep suspension balling-up or one
Suspension balling-up, " adding naphthalene-except naphthalene " are all the indispensable links of suspension method balling-up.But the process of " add naphthalene-except naphthalene " without
It needs the equipment that cover that technical process is lengthened more in shape, while increasing production cost, and be inevitably generated environmental pollution.
(pre-) oxidation technology is to maintain the committed step of bitumen ball pattern, especially in production grade, submillimeter level ball
When shaped activated carbon.The oxidizing gas (mostly air) for industrially generalling use heat is purged, such as patent CN 102795624
A " the low power consuming preparation method of asphalt-base spherical activated carbon "；Described in 1607174 A of CN " method for preparing spherical activated carbon ".
However, its oxidation cycle is all at 30 hours or more, time consumption and energy consumption.
In conclusion it is raw material that the preparation of asphalt-base globular active carbon, which generally selects high softening point bitumen, need through " adding naphthalene-
Except naphthalene " link and slow oxidative stabilization process.Although middle soft pitch has, softening point is low, at low cost, plasticity is strong, no
Need to add naphthalene can low temperature balling-up the features such as, but in all disclosed methods, there is no report uses in soft pitch prepared for raw material
Asphalt-base globular active carbon.
Summary of the invention
For prior art cost of material height, complex process, high pollution, energy consumption is high, oxidation cycle is long the deficiencies of, the present invention
Purpose to be to provide a kind of by middle soft pitch be raw material, be not added naphthalene can balling-up and can quick oxidative stabilization, through carbonizing
To get the preparation method of asphalt-base globular active carbon after activation.Products obtained therefrom, sphericity is good, and intensity is higher, and can scale
Change, consecutive production.
Preparation method of the invention, includes the following steps:
Middle soft pitch raw material and modifying agent are added in reaction kettle, under nitrogen protection, after being heated to 100~300 DEG C
It is stirred, 0.5~4h of constant temperature is subsequently vacuumed out, cooling discharge, the modified pitch that can be used for balling-up is obtained, using being emulsified into
Bitumen ball is made in ball method, and the bitumen ball is then placed directly within the hollow air-blowing of oxidation furnace without any processing and is swept, with 30~60
℃ h-1Heating rate be warming up to 250~350 DEG C, 0.5~4h of constant temperature to get stabilized bitumen ball, and then carbonized-
Activation, can be obtained asphalt-base globular active carbon.
Soft pitch raw material includes that one or more of asphalt, coal tar pitch, bitumen are mixed in as described above
Object is closed, softening point is 40~100 DEG C.
Modifying agent as described above is anhydrous aluminum chloride, anhydrous ferric chloride, anhydrous zinc chloride, anhydrous stannic chloride, borontrifluoride
One or more of boron, metaformaldehyde, p-methyl benzenesulfonic acid, iodine, chloroform and bromofom, and the modifying agent additive amount account in it is low
The 1%~20% of warm asphalt stock quality, preferably 5%~15%.
Emulsification pelletizing method as described above, referring to patent CN 1188074A " a kind of preparation method of spheric active carbon ",
The modified pitch particle of corresponding granularity after sieving is taken to be placed in reaction kettle, what addition was made of surfactant and decentralized medium
Emulsion is 130~150 DEG C in temperature, under 0.4~0.8MPa of pressure, bitumen ball is made by emulsion process.Wherein, surface is living
Property agent can be polyvinyl acetate, methylcellulose, polyethylene glycol, the polyvinyl alcohol of half saponification, and decentralized medium can be silicon
Oil, glycerine, hydro carbons higher-boiling compound, water.
Charcoal-activation as described above is referring to a kind of 106348290 A of patent CN " high-termal conductivity asphalt-base globular active carbon
Preparation method ", i.e., stabilized bitumen ball is placed in activation furnace, with 8~20 DEG C of min-1Heating rate is in an inert atmosphere
From room temperature to 800~1000 DEG C of 0.1~1h of stop, it is switched to vapor or CO later2Activate 1~5h.
Present invention has an advantage that the total of final products can be obviously improved directly using city's mid-sales soft pitch as raw material
Yield, do not need " add naphthalene-except naphthalene " process can balling-up, technique can be reduced to direct balling, and required item when balling-up
Part is mild, significantly reduces the environmental pollution caused by the distillation of naphthalene and causes the unstable of properties of product, gained drip
Green ball, which can be aoxidized directly, not to be melted, is aoxidized the nonfused time and by 30~50h of common process is shortened to the 10 of this patent
~20h.In short, this method have at low cost, simple process, industrialization promotion be easy etc. advantages, prepared spheric active carbon
Sphere diameter is uniform, and sphericity is up to 0.93 or more, 95% or more intensity, 1100~1700m of specific surface area2g-1。
Specific embodiment
The method of the present invention will be further described by several embodiments below.
Embodiment 1
Asphalt (softening point be 45 DEG C) and anhydrous aluminum chloride (additive amount account for oil pitch quality 5%) are mixed equal
It is added in reaction kettle after even, under nitrogen protection, simultaneously constant temperature 3h is stirred after being heated to 150 DEG C, is subsequently vacuumed out, cools down out
Material, obtains the modified pitch (117 DEG C of softening point) that can be used for balling-up, and bitumen ball is made using emulsification pelletizing method, then should
Bitumen ball is placed directly within the hollow air-blowing of oxidation furnace without any processing and sweeps, with 30 DEG C of h-1Heating rate be warming up to 250 DEG C, it is permanent
Warm 1h can be obtained asphalt-base globular active carbon to get stabilized bitumen ball, and then by its charcoal-activation.Prepared ball
Shaped activated carbon uniform particle sizes (average grain diameter 0.8mm), sphericity 0.98, intensity 95%, specific surface area 1100m2g-1。
Embodiment 2
By coal tar pitch (softening point be 80 DEG C) and chloroform (additive amount account for oil pitch quality 10%) after mixing plus
Enter in reaction kettle, under nitrogen protection, simultaneously constant temperature 3.5h be stirred after being heated to 280 DEG C, is subsequently vacuumed out, cooling discharge,
The modified pitch (softening point is 117 DEG C) that can be used for balling-up is obtained, bitumen ball is made using emulsification pelletizing method, then by the drip
Green ball is placed directly within the hollow air-blowing of oxidation furnace without any processing and sweeps, with 60 DEG C of h-1Heating rate be warming up to 290 DEG C, constant temperature
3h can be obtained asphalt-base globular active carbon to get stabilized bitumen ball, and then by its charcoal-activation.Prepared is spherical
Activated carbon particle size is uniform (average grain diameter 0.4mm), sphericity 0.95, intensity 96%, specific surface area 1,220m2g-1。
Embodiment 3
Bitumen (softening point be 60 DEG C) and metaformaldehyde (additive amount account for oil pitch quality 15%) are mixed equal
It is added in reaction kettle after even, under nitrogen protection, simultaneously constant temperature 2h is stirred after being heated to 300 DEG C, is subsequently vacuumed out, cools down out
Material obtains the modified pitch (softening point is 127 DEG C) that can be used for balling-up, bitumen ball is made using emulsification pelletizing method, then will
The bitumen ball is placed directly within the hollow air-blowing of oxidation furnace without any processing and sweeps, with 50 DEG C of h-1Heating rate be warming up to 350 DEG C,
Constant temperature 2h can be obtained asphalt-base globular active carbon to get stabilized bitumen ball, and then by its charcoal-activation.Prepared
Spheric active carbon uniform particle sizes (average grain diameter 0.3mm), sphericity 0.95, intensity 97%, specific surface area 1298m2g-1。
Embodiment 4
Coal tar pitch (softening point be 90 DEG C) and p-methyl benzenesulfonic acid (additive amount account for oil pitch quality 13%) are mixed equal
It is added in reaction kettle after even, under nitrogen protection, simultaneously constant temperature 4h is stirred after being heated to 250 DEG C, is subsequently vacuumed out, cools down out
Material obtains the modified pitch (softening point is 169 DEG C) that can be used for balling-up, bitumen ball is made using emulsification pelletizing method, then will
The bitumen ball is placed directly within the hollow air-blowing of oxidation furnace without any processing and sweeps, with 40 DEG C of h-1Heating rate be warming up to 320 DEG C,
Constant temperature 4h can be obtained asphalt-base globular active carbon to get stabilized bitumen ball, and then by its charcoal-activation.Prepared
Spheric active carbon uniform particle sizes (average grain diameter 0.9mm), sphericity 0.97, intensity 95%, specific surface area 1370m2g-1。
Embodiment 5
Asphalt (softening point be 70 DEG C) and anhydrous ferric chloride (additive amount account for oil pitch quality 8%) are mixed equal
It is added in reaction kettle after even, under nitrogen protection, simultaneously constant temperature 4h is stirred after being heated to 100 DEG C, is subsequently vacuumed out, cools down out
Material obtains the modified pitch (softening point is 130 DEG C) that can be used for balling-up, bitumen ball is made using emulsification pelletizing method, then will
The bitumen ball is placed directly within the hollow air-blowing of oxidation furnace without any processing and sweeps, with 30 DEG C of h-1Heating rate be warming up to 280 DEG C,
Constant temperature 0.5h can be obtained asphalt-base globular active carbon to get stabilized bitumen ball, and then by its charcoal-activation.It is prepared
Spheric active carbon uniform particle sizes (average grain diameter 0.5mm), sphericity 0.94, intensity 98%, specific surface area 1367m2g-1。
Embodiment 6
Bitumen (softening point be 50 DEG C) and anhydrous stannic chloride (additive amount account for oil pitch quality 7%) are mixed equal
It is added in reaction kettle after even, under nitrogen protection, simultaneously constant temperature 0.5h is stirred after being heated to 180 DEG C, is subsequently vacuumed out, is cooled down
Discharging obtains the modified pitch (softening point is 100 DEG C) that can be used for balling-up, bitumen ball is made using emulsification pelletizing method, then
The bitumen ball is placed directly within the hollow air-blowing of oxidation furnace without any processing to sweep, with 30 DEG C of h-1Heating rate be warming up to 260
DEG C, constant temperature 2.5h can be obtained asphalt-base globular active carbon to get stabilized bitumen ball, and then by its charcoal-activation.It is made
Standby spheric active carbon uniform particle sizes (average grain diameter 1.2mm), sphericity 0.98, intensity 96.5%, specific surface area 1588m2g-1。
Embodiment 7
Coal tar pitch (softening point be 100 DEG C) and iodine (additive amount account for oil pitch quality 12%) are added after mixing
In reaction kettle, under nitrogen protection, it is stirred simultaneously constant temperature 2.5h after being heated to 230 DEG C, is subsequently vacuumed out, cooling discharge obtains
To the modified pitch (softening point is 192 DEG C) that can be used for balling-up, bitumen ball is made using emulsification pelletizing method, then by the pitch
Ball is placed directly within the hollow air-blowing of oxidation furnace without any processing and sweeps, with 50 DEG C of h-1Heating rate be warming up to 350 DEG C, constant temperature
3.5h can be obtained asphalt-base globular active carbon to get stabilized bitumen ball, and then by its charcoal-activation.Prepared ball
Shaped activated carbon uniform particle sizes (average grain diameter 1.5mm), sphericity 0.95, intensity 98%, specific surface area 1680m2g-1。
Embodiment 8
By asphalt (softening point is 40 DEG C) and bitumen (softening point is 65 DEG C) (asphalt: bitumen=
3:2 (weight ratio)) co-grinding, after screening with anhydrous aluminum chloride and p-methyl benzenesulfonic acid mixture (anhydrous aluminum chloride: to toluene sulphur
Acid=1:1 (weight ratio), accounts for the 15% of mix asphalt total weight) it is added in reaction kettle together, under nitrogen protection, it is heated to
It is stirred simultaneously constant temperature 3.5h after 200 DEG C, is subsequently vacuumed out, cooling discharge, obtains the modified pitch (softening point that can be used for balling-up
It is 128 DEG C), bitumen ball is made using emulsification pelletizing method, the bitumen ball is then placed directly within oxidation furnace without any processing
Hollow air-blowing is swept, with 40 DEG C of h-1Heating rate be warming up to 340 DEG C, constant temperature 1.5h, and then will to get stabilized bitumen ball
Its charcoal-activation, can be obtained asphalt-base globular active carbon.(average grain diameter is by prepared spheric active carbon uniform particle sizes
1.6mm), sphericity 0.95, intensity 95%, specific surface area 1620m2g-1。
Embodiment 9
By coal tar pitch (softening point is 90 DEG C) and bitumen (softening point is 65 DEG C) (coal tar pitch: bitumen=1:2
(weight ratio)) it co-grinding, is added in reaction kettle together with metaformaldehyde (account for mix asphalt total weight 9%) after screening,
Under nitrogen protection, it is stirred simultaneously constant temperature 1.5h after being heated to 240 DEG C, is subsequently vacuumed out, cooling discharge, obtains can be used for balling-up
Modified pitch (softening point be 150 DEG C), bitumen ball is made using emulsification pelletizing method, then by the bitumen ball without any place
Reason is placed directly within the hollow air-blowing of oxidation furnace and sweeps, with 30 DEG C of h-1Heating rate be warming up to 300 DEG C, constant temperature 0.5h is to get stabilisation
Bitumen ball can be obtained asphalt-base globular active carbon and then by its charcoal-activation.Prepared spheric active carbon uniform particle sizes
(average grain diameter 0.7mm), sphericity 0.94, intensity 95%, specific surface area 1457m2g-1。
Embodiment 10
Coal tar pitch (softening point is 90 DEG C) is crushed, mixture (the anhydrous chlorination after screening with anhydrous aluminum chloride and chloroform
Aluminium: chloroform=1:3 (weight ratio) accounts for the 6% of bitumen total weight) it is added in reaction kettle together, under nitrogen protection, heating
It is stirred simultaneously constant temperature 3h after to 140 DEG C, is subsequently vacuumed out, cooling discharge, obtains the modified pitch (softening point that can be used for balling-up
It is 148 DEG C), bitumen ball is made using emulsification pelletizing method, the bitumen ball is then placed directly within oxidation furnace without any processing
Hollow air-blowing is swept, with 30 DEG C of h-1Heating rate be warming up to 310 DEG C, constant temperature 1h to get stabilized bitumen ball, and then by its
Charcoal-activation, can be obtained asphalt-base globular active carbon.(average grain diameter is by prepared spheric active carbon uniform particle sizes
0.6mm), sphericity 0.98, intensity 96%, specific surface area 1350m2g-1。
Embodiment 11
Asphalt (softening point is 40 DEG C) is crushed, the mixture (nothing after screening with anhydrous ferric chloride and metaformaldehyde
Water iron chloride: metaformaldehyde=1:1 (weight ratio) accounts for the 11% of bitumen total weight) it is added in reaction kettle together, in nitrogen
Under protection, it is stirred simultaneously constant temperature 2h after being heated to 260 DEG C, is subsequently vacuumed out, cooling discharge, obtains the modification that can be used for balling-up
Pitch (softening point is 152 DEG C), is made bitumen ball using emulsification pelletizing method, then that the bitumen ball is direct without any processing
It is placed in the hollow air-blowing of oxidation furnace to sweep, with 40 DEG C of h-1Heating rate be warming up to 330 DEG C, constant temperature 2h to get stabilized bitumen ball,
And then by its charcoal-activation, asphalt-base globular active carbon can be obtained.Prepared spheric active carbon uniform particle sizes' (average grain diameter
For 0.5mm), sphericity 0.94, intensity 95%, specific surface area 1706m2g-1。
Embodiment 12
Bitumen (softening point is 65 DEG C) is crushed, mixture (the anhydrous chlorine after screening with anhydrous zinc chloride and formaldehyde
Change zinc: formaldehyde=3:2 (weight ratio) accounts for the 14% of bitumen total weight) it is added in reaction kettle together, under nitrogen protection,
It is stirred simultaneously constant temperature 1h after being heated to 290 DEG C, is subsequently vacuumed out, cooling discharge, the modified pitch for obtaining can be used for balling-up is (soft
Changing point is 178 DEG C), bitumen ball is made using emulsification pelletizing method, the bitumen ball is then placed directly within oxygen without any processing
Change the hollow air-blowing of furnace to sweep, with 50 DEG C of h-1Heating rate be warming up to 270 DEG C, constant temperature 3h is to get stabilized bitumen ball, in turn
By its charcoal-activation, asphalt-base globular active carbon can be obtained.(average grain diameter is by prepared spheric active carbon uniform particle sizes
1.4mm), sphericity 0.95, intensity 97%, specific surface area 1157m2g-1。
Embodiment 13
By asphalt (softening point is 45 DEG C) and coal tar pitch (softening point is 90 DEG C) (asphalt: coal tar pitch=1:4
(weight ratio)) co-grinding, (chloroform: bromofom=1:1 (weight ratio) accounts for mixing drip with the mixture of chloroform and bromofom after screening
The 10% of green total weight) it is added in reaction kettle together, under nitrogen protection, simultaneously constant temperature 4h is stirred after being heated to 220 DEG C, with
After vacuumize, cooling discharge obtains can be used for the modified pitch (softening point is 154 DEG C) of balling-up, using emulsification pelletizing method system
Bitumen ball is obtained, the bitumen ball is then placed directly within the hollow air-blowing of oxidation furnace without any processing and is swept, with 40 DEG C of h-1Heating speed
Rate is warming up to 300 DEG C, and it is living to can be obtained asphalt-base globular to get stabilized bitumen ball, and then by its charcoal-activation by constant temperature 4h
Property charcoal.Prepared spheric active carbon uniform particle sizes (average grain diameter 1.3mm), sphericity 0.98, intensity 94%, specific surface area
1537m2g-1。
Embodiment 14
By asphalt (softening point is 45 DEG C), coal tar pitch (softening point is 90 DEG C) and bitumen (softening point is 65 DEG C)
After (asphalt: coal tar pitch: bitumen=3:2:1 (weight ratio)) co-grinding, screening with anhydrous aluminum chloride, formaldehyde, chlorine
Imitative mixture (anhydrous aluminum chloride: formaldehyde: chloroform=2:1:2 (weight ratio) accounts for the 15% of mix asphalt total weight) adds together
Enter in reaction kettle, under nitrogen protection, simultaneously constant temperature 3h is stirred after being heated to 270 DEG C, is subsequently vacuumed out, cooling discharge obtains
To the modified pitch (softening point is 165 DEG C) that can be used for balling-up, bitumen ball is made using emulsification pelletizing method, then by the pitch
Ball is placed directly within the hollow air-blowing of oxidation furnace without any processing and sweeps, with 30 DEG C of h-1Heating rate be warming up to 350 DEG C, constant temperature
2.5h can be obtained asphalt-base globular active carbon to get stabilized bitumen ball, and then by its charcoal-activation.Prepared ball
Shaped activated carbon uniform particle sizes (average grain diameter 0.8mm), sphericity 0.94, intensity 96%, specific surface area 1420m2g-1。
Embodiment 15
By asphalt (softening point is 45 DEG C) and coal tar pitch (softening point is 78 DEG C) (asphalt: coal tar pitch=4:3
(weight ratio)) co-grinding, after screening with anhydrous ferric chloride, metaformaldehyde, bromofom mixture (anhydrous ferric chloride: trimerization first
Aldehyde: bromofom=3:1:4 (weight ratio) accounts for the 10% of mix asphalt total weight) it is added in reaction kettle together, under nitrogen protection,
It is stirred simultaneously constant temperature 1.5h after being heated to 170 DEG C, is subsequently vacuumed out, cooling discharge, obtains the modified pitch that can be used for balling-up
(softening point is 128 DEG C) is made bitumen ball using emulsification pelletizing method, is then placed directly within the bitumen ball without any processing
The hollow air-blowing of oxidation furnace is swept, with 30 DEG C of h-1Heating rate be warming up to 340 DEG C, constant temperature 1h to get stabilized bitumen ball, into
And by its charcoal-activation, it can be obtained asphalt-base globular active carbon.(average grain diameter is by prepared spheric active carbon uniform particle sizes
0.9mm), sphericity 0.98, intensity 94%, specific surface area 1510m2g-1。
Claims (6)
1. a kind of method for preparing asphalt-base globular active carbon, it is characterised in that include the following steps:
Middle soft pitch raw material and modifying agent are added in reaction kettle, under nitrogen protection, stirred after being heated to 100~300 DEG C
Mixing, 0.5~4 h of constant temperature are subsequently vacuumed out, cooling discharge, obtain the modified pitch that can be used for balling-up, using emulsification balling-up side
Legal system obtains bitumen ball, and the bitumen ball is then placed directly within the hollow air-blowing of oxidation furnace without any processing and is swept, with 30~60 DEG C of h-1
Heating rate be warming up to 250~350 DEG C, 0.5~4 h of constant temperature is to get stabilized bitumen ball, and then by its charing-work
Change, i.e. acquisition asphalt-base globular active carbon.
2. a kind of method for preparing asphalt-base globular active carbon as described in claim 1, it is characterised in that the middle low temperature
Asphalt stock is one or more of asphalt, coal tar pitch, bitumen mixture, and softening point is 40~100 DEG C.
3. a kind of method for preparing asphalt-base globular active carbon as described in claim 1, it is characterised in that the modifying agent
For anhydrous aluminum chloride, anhydrous ferric chloride, anhydrous zinc chloride, anhydrous stannic chloride, boron trifluoride, metaformaldehyde, p-methyl benzenesulfonic acid,
One or more of iodine, chloroform and bromofom, and modifying agent additive amount accounts for the 1%~20% of middle soft pitch material quality.
4. a kind of method for preparing asphalt-base globular active carbon as described in claim 1, it is characterised in that the modifying agent
Additive amount accounts for the 5%~15% of middle soft pitch material quality.
5. a kind of method for preparing asphalt-base globular active carbon as described in claim 1, it is characterised in that described is emulsified into
Ball method is that the modified pitch particle of corresponding granularity after taking screening is placed in reaction kettle, is added by surfactant and decentralized medium
The emulsion of composition is 130~150 in temperatureoUnder C, 0.4~0.8 MPa of pressure, bitumen ball is made by emulsion process, wherein
Surfactant can be polyvinyl acetate, methylcellulose, polyethylene glycol, the polyvinyl alcohol of half saponification, and decentralized medium can
To be silicone oil, glycerine, hydro carbons higher-boiling compound or water.
6. a kind of method for preparing asphalt-base globular active carbon as described in claim 1, it is characterised in that the charcoal-work
Change is that stabilized bitumen ball is placed in activation furnace, with 8~20 DEG C of min-1Heating rate is in an inert atmosphere from room temperature
To 800~1000 DEG C of stop 0 .1~1h, it is switched to vapor or CO later2Activate 1~5h.
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| CN110482521A (en) * | 2019-07-24 | 2019-11-22 | 厦门大学 | A kind of preparation method of hollow carbon balls |
| CN110540854A (en) * | 2019-09-05 | 2019-12-06 | 中国科学院山西煤炭化学研究所 | Method for preparing asphalt-based oxidation ball |
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| CN112125306A (en) * | 2020-09-28 | 2020-12-25 | 烟台中科恩吉科创新产业园管理有限公司 | Activated carbon and preparation method thereof |
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| CN110482521A (en) * | 2019-07-24 | 2019-11-22 | 厦门大学 | A kind of preparation method of hollow carbon balls |
| CN110482521B (en) * | 2019-07-24 | 2021-04-06 | 厦门大学 | Preparation method of hollow carbon spheres |
| CN110540854A (en) * | 2019-09-05 | 2019-12-06 | 中国科学院山西煤炭化学研究所 | Method for preparing asphalt-based oxidation ball |
| CN111422869A (en) * | 2020-03-04 | 2020-07-17 | 山西新华化工有限责任公司 | Preparation method for industrially improving crushing strength of asphalt balls |
| CN113912059A (en) * | 2020-07-09 | 2022-01-11 | 中国科学院大连化学物理研究所 | Asphalt-based spherical activated carbon and preparation method and application thereof |
| CN113912059B (en) * | 2020-07-09 | 2023-06-06 | 中国科学院大连化学物理研究所 | Asphalt-based spherical activated carbon and preparation method and application thereof |
| CN112125306A (en) * | 2020-09-28 | 2020-12-25 | 烟台中科恩吉科创新产业园管理有限公司 | Activated carbon and preparation method thereof |
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