CN107758661A - A kind of method that petroleum coke for preventing that product from luming prepares active carbon with high specific surface area - Google Patents
A kind of method that petroleum coke for preventing that product from luming prepares active carbon with high specific surface area Download PDFInfo
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- CN107758661A CN107758661A CN201711205721.6A CN201711205721A CN107758661A CN 107758661 A CN107758661 A CN 107758661A CN 201711205721 A CN201711205721 A CN 201711205721A CN 107758661 A CN107758661 A CN 107758661A
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- petroleum coke
- surface area
- specific surface
- active carbon
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Abstract
The invention discloses a kind of method that petroleum coke for preventing that product from luming prepares active carbon with high specific surface area, the loose porous product that preparation is drawn is washed, dried, ground, obtain active carbon with high specific surface area.Product hardens the problem lumpd during efficiently solving petroleum coke and KOH priming reactions, reduces activation temperature, reduces cost, simple to operate.
Description
Technical field
The present invention relates to activated carbon preparing technical field, more particularly to a kind of petroleum coke for preventing that product from luming to prepare high ratio
The method of surface area activated carbon.
Background technology
Petroleum coke is that petroleum chemical industry utilizes coking technology, to mink cell focuses such as decompression residuum, secondary operation tail oils, is carried out
The solid residue left after high temperature deep processing, it is the accessory substance in petroleum refining process, there is high phosphorus content, sulfur height, contain
There is the characteristics of heavy metal compound.For the carbon amounts of petroleum coke typically more than 80%, calorific value also corresponds to 1.5 times of coal.Oil
Contain the elements such as sulphur, nitrogen and heavy metal in burnt the inside.The higher petroleum coke of sulfur content, its SO2 emissions is bigger, right
Environment produces certain negative impact.And petroleum coke as industrial fuel when be mostly the low-quality petroleum coke of high-sulfur, its combustion power generation
Caused atmosphere pollution easily produces considerable influence to environment.How environmental protection treatment petroleum coke, be the sternness currently faced
Environmental problem.The use of preparing absorbent charcoal with petroleum coke is one of which processing mode, but due to petroleum coke be heavy, high-sulfur,
Accessory substance after the crude oil refinery of high metal content, during activated carbon is prepared, product caking phenomenon is serious, to preparing
Journey and final product are negatively affected.
The content of the invention
In view of this, the technical problem to be solved in the present invention is how to provide a kind of petroleum coke system for preventing product from luming
The method of standby active carbon with high specific surface area.
To solve above technical problem, the embodiment of the present invention provides a kind of petroleum coke for preventing product from luming and prepares Gao Bibiao
The method of area activated carbon, comprises the following steps：
Step S1, by petroleum coke, soda ash and deionized water according to mass ratio 1：2~4：0.8~1 ratio mixing, leaching
10~15h, 0.5~1.5h of ultrasonic vibration are steeped, is heated with stirring to 120~150 DEG C in closed container, separation of solid and liquid is then carried out and takes off
Silicon, leave and take solid and obtain the first product；
Step S2, inorganic acid mixed solution is added to the first product, soaks 5~7h, 0.5~1.5h of closed stirring, then
Separation of solid and liquid is carried out, solid is left and taken and obtains the second product；Wherein, the inorganic acid mixed solution is：50~80wt% of watery hydrochloric acid,
5~40wt% of phosphoric acid, 5~20wt% of hypochlorous acid；
Step S3, after second product being washed into neutrality, in 95~105 DEG C of dry third products；
Step S4, KOH and KNO is added in the third product3, the first mixture is obtained after being sufficiently stirred；Wherein, institute
State third product, KOH, KNO3 mass ratio are 1：1~2.5：0.5~1；
Step S5, by first mixture, step heating, the first step are warming up to 300~400 in mixed inert atmosphere
DEG C, 1~3h of heat time；Second step is warming up to 400~600 DEG C, 1~3h of heat time, obtains loose porous product；Wherein,
The mixed inert atmosphere volume ratio is：Argon gas 35~80%, nitrogen 20~65%, the mixed inert atmosphere pressure are
0.09~0.12mpa；
Step S6, the loose porous product is washed, dried, ground, obtain active carbon with high specific surface area.
Preferably, the method that the petroleum coke provided by the invention for preventing that product from luming prepares active carbon with high specific surface area, step
In rapid S5, the heating rate of the first step heating is 5~15 DEG C/min.
Preferably, the method that the petroleum coke provided by the invention for preventing that product from luming prepares active carbon with high specific surface area, step
In rapid S5, the heating rate of the second step heating is 3~7 DEG C/min.
Preferably, the method that the petroleum coke provided by the invention for preventing that product from luming prepares active carbon with high specific surface area, institute
The petroleum coke stated is delay Jiao and/or fluid coke.
Preferably, the method that the petroleum coke provided by the invention for preventing that product from luming prepares active carbon with high specific surface area, bag
Include：
Step S1, by petroleum coke, soda ash and deionized water according to mass ratio 1：2~3：1 ratio mixing, soaks 12h,
Ultrasonic vibration 1h, 150 DEG C are heated with stirring in closed container, then carry out separation of solid and liquid desiliconization, leave and take solid and obtain the first production
Thing；
Step S2, inorganic acid mixed solution is added to the first product, soaks 6h, closed stirring 1h, then carry out solid-liquid point
From leaving and taking solid and obtain the second product；
Step S3, after second product being washed into neutrality, in 100 DEG C of dry third products；
Step S4, KOH and KNO is added in the third product3, the first mixture is obtained after being sufficiently stirred；Wherein, institute
State third product, KOH, KNO3 mass ratio are 1：1~1.5：0.8~1；
Step S5, by first mixture, step heating, the first step are warming up to 350 DEG C, added in mixed inert atmosphere
Hot time 2h；Second step is warming up to 500 DEG C, heat time 2h, obtains loose porous product；Wherein, the mixed inert atmosphere
Volume ratio is：Argon gas 80%, nitrogen 20%, the mixed inert atmosphere pressure are 0.09~0.12mpa；
Step S6, the loose porous product is washed, dried, ground, obtain active carbon with high specific surface area.
Thus, it is an advantage of the invention that solving the problem of product hardening caking during petroleum coke and KOH priming reactions,
Activation temperature is reduced, reduces cost, it is simple to operate.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in the embodiment of the present invention
Technical scheme is clearly and completely described, it is clear that and described embodiment is part of the embodiment of the present invention, rather than entirely
The embodiment in portion.Based on the embodiment in the present invention, those of ordinary skill in the art are not under the premise of creative work is made
The every other embodiment obtained, belongs to the scope of protection of the invention.Explicitly indicated that unless otherwise other, otherwise whole
In specification and claims, term " comprising " or its conversion such as "comprising" or " including " etc. will be understood to comprise institute
The element or part of statement, and do not exclude other elements or other parts.
Special word " exemplary " is meant " being used as example, embodiment or illustrative " herein.Here as " exemplary "
Illustrated any embodiment should not necessarily be construed as preferred or advantageous over other embodiments.
In addition, in order to better illustrate the present invention, numerous details is given in embodiment below.
It will be appreciated by those skilled in the art that without some details, the present invention can equally be implemented.In some instances, for
Method well known to those skilled in the art, means, element are not described in detail, in order to highlight the purport of the present invention.
Embodiment 1
By petroleum coke, soda ash and deionized water according to mass ratio 1：2：1 ratio mixing, soaks 15h, ultrasonic vibration
1h, 150 DEG C are heated with stirring in closed container, then carry out separation of solid and liquid desiliconization, leave and take solid and obtain the first product；To first
Product adds inorganic acid mixed solution, soaks 5h, closed stirring 1h, then carries out separation of solid and liquid, leave and take solid and obtain the second production
Thing；Wherein, the inorganic acid mixed solution is：Watery hydrochloric acid 50wt%, phosphoric acid 30wt%, hypochlorous acid 20wt%；By described second
After product is washed to neutrality, in 105 DEG C of dry third products；KOH and KNO is added in the third product3, it is sufficiently stirred
After obtain the first mixture；Wherein, the third product, KOH, KNO3 mass ratio are 1：1：1；By first mixture mixed
Step heating in inert atmosphere is closed, the first step is warming up to 300 DEG C, and heating rate is 10 DEG C/min；Heat time 2h；Second step liter
For temperature to 500 DEG C, heating rate is 5 DEG C/min, heat time 1h, obtains loose porous product；Wherein, the mixed inert atmosphere
Volume ratio is：Argon gas 80%, nitrogen 20%, the mixed inert atmosphere pressure are 0.09~0.12mpa；Will be described loose more
Hole product is washed, dried, and grinding, obtains active carbon with high specific surface area.In preparation process, do not find that product hardening caking is existing
As.Final product active carbon with high specific surface area does not find to harden caking phenomenon.
Embodiment 2
By petroleum coke, soda ash and deionized water according to mass ratio 1：2.5：0.8 ratio mixing, soak 10h, ultrasound shake
1.5h is swung, 120 DEG C are heated with stirring in closed container, separation of solid and liquid desiliconization is then carried out, leaves and takes solid and obtain the first product；To
First product adds inorganic acid mixed solution, soaks 5h, closed stirring 0.5h, then carries out separation of solid and liquid, leave and take solid and obtain
Second product；Wherein, the inorganic acid mixed solution is：Watery hydrochloric acid 60wt%, phosphoric acid 20wt%, hypochlorous acid 20wt%；By institute
State after the second product is washed to neutrality, in 100 DEG C of dry third products；KOH and KNO is added in the third product3, fill
The first mixture is obtained after dividing stirring；Wherein, the third product, KOH, KNO3 mass ratio are 1：2：0.5；Described first is mixed
Compound step heating in mixed inert atmosphere, the first step are warming up to 350 DEG C, and heating rate is 8~10 DEG C/min, reach temperature
After heat 1h；Second step is warming up to 600 DEG C, and heating rate is 7 DEG C/min, heats 2h after reaching temperature, obtains loose porous production
Thing；Wherein, the mixed inert atmosphere volume ratio is：Argon gas 50%, nitrogen 50%, the mixed inert atmosphere pressure are
0.09~0.12mpa；The loose porous product is washed, dried, grinds, obtains active carbon with high specific surface area.This reality
Apply in example, petroleum coke is burnt using delay.In preparation process, do not find that product hardens caking phenomenon.Final product high-specific surface area
Activated carbon does not find to harden caking phenomenon.
Embodiment 3
By petroleum coke, soda ash and deionized water according to mass ratio 1：4：0.8 ratio mixing, soaks 10h, ultrasonic vibration
0.5h, 150 DEG C are heated with stirring in closed container, then carry out separation of solid and liquid desiliconization, leave and take solid and obtain the first product；To
One product adds inorganic acid mixed solution, soaks 7h, closed stirring 1.5h, then carries out separation of solid and liquid, leaves and takes solid and obtains the
Two products；Wherein, the inorganic acid mixed solution is：Watery hydrochloric acid 80wt%, phosphoric acid 5wt%, hypochlorous acid 15wt%；By described
After two products are washed to neutrality, in 95 DEG C of dry third products；KOH and KNO is added in the third product3, fully stir
The first mixture is obtained after mixing；Wherein, the third product, KOH, KNO3 mass ratio are 1：2.5：0.5；Described first is mixed
Thing step heating in mixed inert atmosphere, the first step are warming up to 400 DEG C, and heating rate is 15 DEG C/min, add after reaching temperature
Hot 3h；Second step is warming up to 450 DEG C, and heating rate is 5 DEG C/min, heats 1h after reaching temperature, obtains loose porous product；Its
In, the mixed inert atmosphere volume ratio is：Argon gas 35%, nitrogen 65%, the mixed inert atmosphere pressure be 0.09~
0.12mpa；The loose porous product is washed, dried, grinds, obtains active carbon with high specific surface area.In the present embodiment,
Petroleum coke uses fluid coke.In preparation process, do not find that product hardens caking phenomenon.Final product active carbon with high specific surface area is not
It was found that hardening caking phenomenon.
Embodiment 4
By petroleum coke, soda ash and deionized water according to mass ratio 1：3：1 ratio mixing, soaks 10h, ultrasonic vibration
0.5h, 120 DEG C are heated with stirring in closed container, then carry out separation of solid and liquid desiliconization, leave and take solid and obtain the first product；To
One product adds inorganic acid mixed solution, soaks 5h, closed stirring 0.5h, then carries out separation of solid and liquid, leaves and takes solid and obtains the
Two products；Wherein, the inorganic acid mixed solution is：Watery hydrochloric acid 70wt%, phosphoric acid 25wt%, hypochlorous acid 5wt%；By described
After two products are washed to neutrality, in 100 DEG C of dry third products；KOH and KNO is added in the third product3, fully stir
The first mixture is obtained after mixing；Wherein, the third product, KOH, KNO3 mass ratio are 1：1：0.5；By first mixture
The step heating in mixed inert atmosphere, the first step are warming up to 300 DEG C, and heating rate is 10 DEG C/min, are heated after reaching temperature
1h；Second step is warming up to 400 DEG C, and heating rate is 5 DEG C/min, heats 1h after reaching temperature, obtains loose porous product；Its
In, the mixed inert atmosphere volume ratio is：Argon gas 70%, nitrogen 30%, the mixed inert atmosphere pressure be 0.09~
0.12mpa；The loose porous product is washed, dried, grinds, obtains active carbon with high specific surface area.In preparation process,
Do not find that product hardens caking phenomenon.Final product active carbon with high specific surface area does not find to harden caking phenomenon.
Embodiment 5
By petroleum coke, soda ash and deionized water according to mass ratio 1：2：1 ratio mixing, soaks 12h, ultrasonic vibration
1h, 150 DEG C are heated with stirring in closed container, then carry out separation of solid and liquid desiliconization, leave and take solid and obtain the first product；To first
Product adds inorganic acid mixed solution, soaks 6h, closed stirring 1h, then carries out separation of solid and liquid, leave and take solid and obtain the second production
Thing；After second product is washed into neutrality, in 100 DEG C of dry third products；In the third product add KOH and
KNO3, the first mixture is obtained after being sufficiently stirred；Wherein, the third product, KOH, KNO3 mass ratio are 1：1.5：0.8；Will
First mixture step heating in mixed inert atmosphere, the first step are warming up to 350 DEG C, and heating rate is 8~10 DEG C/
Min, 2h is heated after reaching temperature；Second step is warming up to 500 DEG C, and heating rate is 5 DEG C/min, heats 2h after reaching temperature, obtains
To loose porous product；Wherein, the mixed inert atmosphere volume ratio is：Argon gas 80%, nitrogen 20%, the mixed inert
Atmosphere pressure is 0.09~0.12mpa；The loose porous product is washed, dried, is ground, obtains high-specific surface area work
Property charcoal.In preparation process, do not find that product hardens caking phenomenon.Final product active carbon with high specific surface area does not find hardening caking
Phenomenon.
The activated carbon obtained to embodiment carries out performance test, as a result as follows：
| Embodiment | Specific surface area m2/g | Iodine sorption value mg/g | Product hardening caking |
| 1 | 4122 | 2330 | Do not find |
| 2 | 3990 | 2502 | Do not find |
| 3 | 4083 | 2411 | Do not find |
| 4 | 4110 | 2270 | Do not find |
| 5 | 4311 | 2381 | Do not find |
Activated carbon prepared by this method, its specific surface area is high, and iodine sorption value is high, has good performance.The present invention provides
Preparation method, solve the problem of product hardening caking during petroleum coke and KOH priming reactions, reduce activation temperature,
Cost is reduced, it is simple to operate.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those within the art that：It still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic；
And these modification or replace, do not make appropriate technical solution essence depart from various embodiments of the present invention technical scheme spirit and
Scope.
Claims (6)
1. a kind of method that petroleum coke for preventing that product from luming prepares active carbon with high specific surface area, it is characterised in that including following
Step：
Step S1, by petroleum coke, soda ash and deionized water according to mass ratio 1：2~4：0.8~1 ratio mixing, immersion 10
~15h, 0.5~1.5h of ultrasonic vibration, 120~150 DEG C are heated with stirring in closed container, then carry out separation of solid and liquid desiliconization,
Leave and take solid and obtain the first product；
Step S2, inorganic acid mixed solution is added to the first product, soaks 5~7h, 0.5~1.5h of closed stirring, then carry out
Separation of solid and liquid, leave and take solid and obtain the second product；Wherein, the inorganic acid mixed solution is：50~80wt% of watery hydrochloric acid, phosphoric acid
5~40wt%, 5~20wt% of hypochlorous acid；
Step S3, after second product being washed into neutrality, in 95~105 DEG C of dry third products；
Step S4, KOH and KNO is added in the third product3, the first mixture is obtained after being sufficiently stirred；Wherein, described
Three products, KOH, KNO3 mass ratio are 1：1~2.5：0.5~1；
Step S5, by first mixture, step heating, the first step are warming up to 300~400 DEG C, added in mixed inert atmosphere
Hot 1~3h of time；Second step is warming up to 400~600 DEG C, 1~3h of heat time, obtains loose porous product；Wherein, it is described mixed
Closing inert atmosphere volume ratio is：Argon gas 35~80%, nitrogen 20~65%, the mixed inert atmosphere pressure be 0.09~
0.12mpa；
Step S6, the loose porous product is washed, dried, ground, obtain active carbon with high specific surface area.
2. the method that the petroleum coke according to claim 1 for preventing that product from luming prepares active carbon with high specific surface area, it is special
Sign is, in step S5, the mixed inert atmosphere volume ratio is：Argon gas 80%, nitrogen 20%, the mixed inert atmosphere
Pressure is 0.09~0.12mpa.
3. the method that the petroleum coke according to claim 1 for preventing that product from luming prepares active carbon with high specific surface area, it is special
Sign is, in step S5, the heating rate of the first step heating is 5~15 DEG C/min.
4. the method that the petroleum coke according to claim 1 for preventing that product from luming prepares active carbon with high specific surface area, it is special
Sign is, in step S5, the heating rate of the second step heating is 3~7 DEG C/min.
5. the petroleum coke according to any one of claims 1 to 4 for preventing that product from luming prepares the side of active carbon with high specific surface area
Method, it is characterised in that described petroleum coke is delay Jiao and/or fluid coke.
6. the method that the petroleum coke according to claim 5 for preventing that product from luming prepares active carbon with high specific surface area, it is special
Sign is, including：
Step S1, by petroleum coke, soda ash and deionized water according to mass ratio 1：2~3：1 ratio mixing, soaks 12h, ultrasound
1h is shaken, 150 DEG C are heated with stirring in closed container, separation of solid and liquid desiliconization is then carried out, leaves and takes solid and obtain the first product；
Step S2, inorganic acid mixed solution is added to the first product, soaks 6h, closed stirring 1h, then carry out separation of solid and liquid, stay
Solid is taken to obtain the second product；
Step S3, after second product being washed into neutrality, in 100 DEG C of dry third products；
Step S4, KOH and KNO is added in the third product3, the first mixture is obtained after being sufficiently stirred；Wherein, described
Three products, KOH, KNO3 mass ratio are 1：1~1.5：0.8~1；
Step S5, by first mixture, step heating, the first step are warming up to 350 DEG C in mixed inert atmosphere, during heating
Between 2h；Second step is warming up to 500 DEG C, heat time 2h, obtains loose porous product；Wherein, the mixed inert atmosphere volume
Ratio is：Argon gas 80%, nitrogen 20%, the mixed inert atmosphere pressure are 0.09~0.12mpa；
Step S6, the loose porous product is washed, dried, ground, obtain active carbon with high specific surface area.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4082694A (en) * | 1975-12-24 | 1978-04-04 | Standard Oil Company (Indiana) | Active carbon process and composition |
| CN103072985A (en) * | 2013-01-10 | 2013-05-01 | 大连理工大学 | Continuous alkali activation device and method for preparing activated carbon with high specific surface area |
| CN105399095A (en) * | 2015-12-28 | 2016-03-16 | 大连理工大学 | Apparatus and method for preparing high specific surface area active carbon through alkali activation process |
-
2017
- 2017-11-27 CN CN201711205721.6A patent/CN107758661A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4082694A (en) * | 1975-12-24 | 1978-04-04 | Standard Oil Company (Indiana) | Active carbon process and composition |
| CN103072985A (en) * | 2013-01-10 | 2013-05-01 | 大连理工大学 | Continuous alkali activation device and method for preparing activated carbon with high specific surface area |
| CN105399095A (en) * | 2015-12-28 | 2016-03-16 | 大连理工大学 | Apparatus and method for preparing high specific surface area active carbon through alkali activation process |
Non-Patent Citations (1)
| Title |
|---|
| 和晓才 等: "从工业石油焦中脱除硅、铝、硫的试验研究", 《湿法冶金》 * |
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Application publication date: 20180306 |