CN105712347B - The method that sulfur-rich activated carbon is prepared using high sulfur petroleum coke - Google Patents
The method that sulfur-rich activated carbon is prepared using high sulfur petroleum coke Download PDFInfo
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- CN105712347B CN105712347B CN201610249895.1A CN201610249895A CN105712347B CN 105712347 B CN105712347 B CN 105712347B CN 201610249895 A CN201610249895 A CN 201610249895A CN 105712347 B CN105712347 B CN 105712347B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention discloses a kind of method that sulfur-rich activated carbon is prepared with high sulfur petroleum coke, comprises the following steps：(10) raw material is mixed：Potassium hydroxide solid powder is mixed with high sulfur petroleum coke particle by proportioning, stirred；(20) calcining and activating：By mixture calcining and activating, the hydrogen sulfide gas produced during calcining and activating is collected, solid is cooled down, washes, dried, and obtains powdered active carbon；(30) petroleum coke combustion：Other burning high sulfur petroleum coke particles, generate sulfur dioxide gas；(40) elemental sulfur is generated：Hydrogen sulfide gas is mixed with sulfur dioxide gas, reaction obtains elemental sulfur；(50) carbon granule impregnates：Activated carbon granule is impregnated in the dipping solution prepared by elemental sulfur after 0.1~72 hour, dries, obtains sulfur-rich activated carbon.The method of the present invention, can be greatly reduced the manufacturing cost of activated carbon, and pollution of the reduction high sulfur petroleum coke to environment reaches the purpose of " Gu sulphur demercuration ".
Description
Technical field
The invention belongs to high sulfur petroleum coke utilization technology field, particularly one kind is prepared sulfur-rich using high sulfur petroleum coke
The method of activated carbon.
Background technology
In recent years, China's rapid economic development, electricity needs is significantly increased so that be used as the coal of the main primary energy of China
Charcoal demand steeply rises.However, a large amount of utilize of coal proposes huge challenge to environmental protection.The constituent of coal is answered
It is miscellaneous, the flue gas containing a large amount of particulate matters, dust, pernicious gas and trace element etc. can be produced when it largely burns, to environment and
Health has serious harm.Wherein the harm of trace element is increasingly paid attention to by people, and mercury is used as most harmful member in coal
One of element, even if aggregate amount very little, can also cause huge harm to ecological environment and human health.Therefore, flue gas demercuration exists
Universal attention is obtained for both at home and abroad.
In numerous demercuration method at present, absorption method demercuration is more effective and more promising controls mercury technology.It is used
Adsorbent mainly includes：Activated carbon, zeolite, calcium matrix activated carbon and flying dust etc..Activated carbon is removed and endangered for being most difficult in flue gas
Great gaseous elemental mercury has good adsorption effect.But commercial activated carbons utilization rate is low, consumption big, directly using activated carbon
Absorption method cost is too high.
Therefore, the problem of prior art is present be：Activated carbon cost for absorption method demercuration is high.
The content of the invention
It is an object of the invention to provide a kind of method that sulfur-rich activated carbon is prepared with high sulfur petroleum coke, activity is greatly reduced
The manufacturing cost of charcoal, while reducing pollution of the high sulfur petroleum coke to environment.
The technical solution for realizing the object of the invention is：
A kind of method that utilization high sulfur petroleum coke prepares sulfur-rich activated carbon, comprises the following steps：
(10) raw material is mixed：It is the high-sulfur of 60~120 mesh, sulfur content higher than 4% by potassium hydroxide solid powder and particle diameter
Petroleum coke particles are mixed by proportioning, are stirred；
Preferably, the mass ratio of high sulfur petroleum coke and potassium hydroxide is 1:3~8, most preferably 1:5.
(20) calcining and activating：By potassium hydroxide and high sulfur petroleum coke granulate mixture calcining and activating 3 at 500~800 DEG C
~6 hours, the hydrogen sulfide gas produced during calcining and activating is collected, solid is cooled to after room temperature and taken out, and through washing, dries,
Obtain powdered active carbon；
Preferably, calcining and activating temperature is 600 DEG C, and the time is 4 hours.
(30) petroleum coke combustion：Other burning high sulfur petroleum coke particles, activation energy is provided for (20) calcining and activating step, is received
Collect the sulfur dioxide gas of generation；
(40) elemental sulfur is generated：Hydrogen sulfide gas is mixed with sulfur dioxide gas, reaction obtains elemental sulfur；
(50) carbon granule impregnates：Activated carbon granule is impregnated in the dipping solution prepared by elemental sulfur after 0.1~72 hour,
Dry, obtain sulfur-rich activated carbon.
Preferably, dipping temperature is 25~100 DEG C；Dip time is 0.1~25 hour；The mass concentration of dipping solution is
1%~50%；Drying temperature is 60~180 DEG C, and drying time is 2~20 hours.
Compared with prior art, its remarkable advantage is the present invention：
The manufacturing cost of activated carbon is greatly reduced, while reducing pollution of the high sulfur petroleum coke to environment.The present invention is using low
It is presoma to be worth discarded object high sulfur petroleum coke, and the method activated with potassium hydroxide base prepares high-ratio surface, high absorption demercuration and used
Activated carbon, the hydrogen sulfide gas produced using activation process and high sulfur petroleum coke are directly burnt the sulfur dioxide gas precursor reactant of generation
Elemental sulfur is generated, elemental sulfur is carried on into activated carbon surface further improves its absorption demercuration ability, reduces the system of activated carbon
Standby cost.While high sulfur petroleum coke recycling and high value added utilization is realized, when reducing high sulfur petroleum coke burning
The sulphur pollution caused.
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Brief description of the drawings
Fig. 1 prepares the method flow diagram of sulfur-rich activated carbon for the present invention using high sulfur petroleum coke.
Fig. 2 prepares the process chart of sulfur-rich activated carbon for the present invention using high sulfur petroleum coke.
Embodiment
Following embodiment is carried out using the step identical with above-mentioned technical proposal, in order to contrast.
Material, equipment used in each embodiment are commercially available without special instruction.Detection method without special instruction be
Conventional method.
Embodiment one
60 mesh high sulfur petroleum cokes are chosen, are in mass ratio 1:5 weigh potassium hydroxide, mix.Mixture is at 600 DEG C
Calcining and activating 3 hours, is cooled to after room temperature and takes out, and obtains powdered active carbon product after washing, drying, collects calcining and activating
During the hydrogen sulfide gas that produces.Choose high sulfur petroleum coke directly to burn, collect the sulfur dioxide gas produced in combustion process
Body.Two kinds of gas mixings are reacted, elemental sulfur product is obtained.Elemental sulfur is configured to the maceration extract that mass concentration is 10%, will
Activated carbon impregnates 3 hours.After the completion of dipping, dried 3 hours in 60 DEG C, sulfur-rich activated carbon is made.Demercuration rate is up to 91%.
Embodiment two
60 mesh high sulfur petroleum cokes are chosen, are in mass ratio 1:5 weigh potassium hydroxide, mix.Mixture is at 600 DEG C
Calcining and activating 4 hours, is cooled to room temperature taking-up, obtains powdered active carbon product after washing, drying, collects calcining and activating mistake
The hydrogen sulfide gas produced in journey.Choose high sulfur petroleum coke directly to burn, collect the sulfur dioxide gas produced in combustion process.
Two kinds of gas mixings are reacted, elemental sulfur product is obtained.Elemental sulfur is configured to the maceration extract that mass concentration is 20%, by activity
Charcoal impregnates 3 hours.After the completion of dipping, dried 4 hours in 80 DEG C, sulfur-rich activated carbon is made.Demercuration rate is up to 95%.
Embodiment three
80 mesh high sulfur petroleum cokes are chosen, are in mass ratio 1:5 weigh potassium hydroxide, mix.Mixture is at 600 DEG C
Calcining and activating 3 hours, is cooled to room temperature taking-up, obtains powdered active carbon product after washing, drying, collects calcining and activating mistake
The hydrogen sulfide gas produced in journey.Choose high sulfur petroleum coke directly to burn, collect the sulfur dioxide gas produced in combustion process.
Two kinds of gas mixings are reacted, elemental sulfur product is obtained and elemental sulfur is configured to the maceration extract that mass concentration is 30%, by activity
Charcoal impregnates 2 hours.After the completion of dipping, dried 6 hours in 80 DEG C, sulfur-rich activated carbon is made.Demercuration rate is up to 93%.
Example IV
100 mesh high sulfur petroleum cokes are chosen, are in mass ratio 1:5 weigh potassium hydroxide, mix.Mixture is at 600 DEG C
Lower calcining and activating 3 hours, is cooled to room temperature taking-up, obtains powdered active carbon product after washing, drying, collects calcining and activating
During the hydrogen sulfide gas that produces.Choose high sulfur petroleum coke directly to burn, collect the sulfur dioxide gas produced in combustion process
Body.Two kinds of gas mixings are reacted, elemental sulfur product is obtained.Elemental sulfur is configured to the maceration extract that mass concentration is 20%, will
Activated carbon impregnates 3 hours.After the completion of dipping, dried 4 hours in 80 DEG C, sulfur-rich activated carbon is made.Demercuration rate is up to 91%.
Embodiment five
120 mesh high sulfur petroleum cokes are chosen, are in mass ratio 1:5 weigh potassium hydroxide, mix.Mixture is at 600 DEG C
Lower calcining and activating 3 hours, is cooled to room temperature taking-up, obtains powdered active carbon product after washing, drying, collects calcining and activating
During the hydrogen sulfide gas that produces.Choose high sulfur petroleum coke directly to burn, collect the sulfur dioxide gas produced in combustion process
Body.Two kinds of gas mixings are reacted, elemental sulfur product is obtained.Elemental sulfur is configured to the maceration extract that mass concentration is 40%, will
Activated carbon impregnates 3 hours.After the completion of dipping, dried 5 hours in 120 DEG C, sulfur-rich activated carbon is made.Demercuration rate is up to 90%.
Claims (7)
1. a kind of method that utilization high sulfur petroleum coke prepares sulfur-rich activated carbon, it is characterised in that comprise the following steps：
(10) raw material is mixed：It is the high-sulfur oil of 60~120 mesh, sulfur content higher than 4% by potassium hydroxide solid powder and particle diameter
Burnt particle is mixed by proportioning, is stirred；
(20) calcining and activating：By potassium hydroxide, the calcining and activating 3~6 at 500~800 DEG C is small with high sulfur petroleum coke granulate mixture
When, the hydrogen sulfide gas produced during calcining and activating is collected, solid is cooled to after room temperature and taken out, and through washing, dries, obtains powder
Last shaped activated carbon；
(30) petroleum coke combustion：Other burning high sulfur petroleum coke particles, activation energy is provided for (20) calcining and activating step, collects life
Into sulfur dioxide gas；
(40) elemental sulfur is generated：Hydrogen sulfide gas is mixed with sulfur dioxide gas, reaction obtains elemental sulfur；
(50) carbon granule impregnates：Activated carbon granule is impregnated in the dipping solution prepared by elemental sulfur after 0.1~72 hour, done
It is dry, obtain sulfur-rich activated carbon；
In (10) the raw material blend step, the mass ratio of high sulfur petroleum coke and potassium hydroxide is 1:3~8.
2. the method according to claim 1 for preparing sulfur-rich activated carbon, it is characterised in that (10) the raw material blend step
In, the mass ratio of high sulfur petroleum coke and potassium hydroxide is 1:5.
3. the method according to claim 1 for preparing sulfur-rich activated carbon, it is characterised in that (20) the calcining and activating step
In, calcining and activating temperature is 600 DEG C, and the time is 4 hours.
4. the method according to claim 1 for preparing sulfur-rich activated carbon, it is characterised in that (50) the carbon granule impregnation steps
In, dipping temperature is 25~100 DEG C.
5. the method according to claim 1 for preparing sulfur-rich activated carbon, it is characterised in that (50) the carbon granule impregnation steps
In, dip time is 0.1~25 hour.
6. the method according to claim 1 for preparing sulfur-rich activated carbon, it is characterised in that (50) the carbon granule impregnation steps
In, the mass concentration of dipping solution is 1%~50%.
7. the method according to claim 1 for preparing sulfur-rich activated carbon, it is characterised in that (50) the carbon granule impregnation steps
In, drying temperature is 60~180 DEG C, and drying time is 2~20 hours.
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| CN107051391A (en) * | 2017-06-29 | 2017-08-18 | 安徽天顺环保设备股份有限公司 | One kind carries the sulfur-rich activated carbon flue gas demercuration adsorbent of bromine and preparation method |
| CN110783553A (en) * | 2019-11-26 | 2020-02-11 | 长虹格兰博科技股份有限公司 | Lithium ion battery anode material and preparation method thereof |
| CN113120901B (en) * | 2019-12-31 | 2023-01-10 | 中国石油化工股份有限公司 | Method for co-producing activated carbon and calcium oxide from petroleum coke and gypsum |
| CN114100592B (en) * | 2021-11-24 | 2023-07-18 | 中南大学 | Method for regenerating flue gas mercury removal material and recovering elemental mercury |
| CN115282951A (en) * | 2022-07-18 | 2022-11-04 | 昆明理工大学 | Modification method of activated carbon for recovering gold in aqueous solution of thiosulfate |
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