CN1076006C - Petroleum asphalt based active carbon and its prepn. method - Google Patents

Petroleum asphalt based active carbon and its prepn. method Download PDF

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Publication number
CN1076006C
CN1076006C CN97101542A CN97101542A CN1076006C CN 1076006 C CN1076006 C CN 1076006C CN 97101542 A CN97101542 A CN 97101542A CN 97101542 A CN97101542 A CN 97101542A CN 1076006 C CN1076006 C CN 1076006C
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China
Prior art keywords
gac
preparation
refinery coke
binding agent
coke
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Expired - Fee Related
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CN97101542A
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CN1189453A (en
Inventor
董兆德
全瀛寰
高利平
侯胜秀
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Dushanzi Petrochemical Plant of Xinjiang Petroleum Administration Bureau
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Dushanzi Petrochemical Plant of Xinjiang Petroleum Administration Bureau
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Abstract

The present invention relates to active carbon which is prepared from petroleum coke prepared from petroleum pitch, a carbon modulating agent for a pore diameter structure and a binding agent. After being pulverized and sieved, the petroleum coke is mixed with the carbon modulating agent for a pore diameter structure and the binding agent according to a proportion. The active carbon is prepared by stirring kneading, formation, carbonization, activation, etc. The active carbon has good absorption performance; the active carbon can be used for various kinds of water treatment and air purification. The method has the advantages of low price and easy acquirement of raw materials and little pollution to environment in preparation processes.

Description

Petroleum asphalt based active carbon and preparation method thereof
The present invention relates to a kind of gac and preparation method thereof, particularly is gac of feedstock production and preparation method thereof with petroleum pitch.
Gac widespread use in industrial and agricultural production and in the daily life, it is varied to make the gac raw material, comprising ature of coal charcoal, carbo lignius and petroleum pitch matter charcoal.Chinese patent application number is that the denomination of invention of 93120049.0 and 93120925.0, two patent applications is " method for preparation of active carbon ".The disclosed major technique feature of application number 93120049.0 patent applications is to be after anti-fusing, carbonization and activation treatment, can obtain activated carbon product with being broken into mixing moulding such as powdered pitch and extrusion aid, tackiness agent.The disclosed major technique of application number 93120925.0 patent applications is characterised in that and will be broken into powdered pitch, through mixing moulding such as anti-fusing back and extrusion aid, tackiness agents; Carry out charing and activation treatment then and can obtain activated carbon product.Anti-melting process has all successively been adopted in above-mentioned two patent applications, and promptly material will heat up 0.1 ℃-1 ℃/minute of heat-up rate gradually in oxidizing atmosphere.This is difficult to control in industrial production, produce comparatively difficulty on industrialized unit, and pitch at high temperature, is discharged many light hydrocarbons and objectionable impurities and is unfavorable for environmental protection when charing, activation procedure in addition.
The objective of the invention is to overcome the shortcoming of prior art, utilize the existing processing unit (plant) of refinery, a kind of technology is simple, easy to operate, pollution is little, product performance are good gac and manufacture method thereof are provided.
Technical characterictic of the present invention is: the refinery coke that this gac is made by petroleum pitch, the modulation agent of carbonaceous aperture structure and binding agent are formed, and the weight % content of each component is as follows:
Refinery coke 30%~80%
Carbonaceous aperture structure modulation agent 0%~30%
Binding agent 10%~35%
Refinery coke recited above is to be made by petroleum pitch, and the weight % content of each component is respectively in the petroleum pitch:
Stable hydrocarbon 10%~70%
Aromatic hydrocarbon 20%~50%
Colloid 5%~30%
Bituminous matter 0.1%~2.5%
The agent of described carbonaceous aperture structure modulation is coal, graphite, starch, charcoal.
Described binding agent is petroleum pitch or coal tar, and it consists of, and aromatic hydrocarbons+colloid+bitum total content is at 45%-70%, and moisture is less than 5%.
The preparation method of petroleum asphalt based active carbon comprises the steps: successively
A. pre-charing operation is industrial vacuum residuum or cracking of ethylene residual oil, catalytic slurry, the extraction wet goods of being referred to as with petroleum pitch, and delayed coking process generates refinery coke;
B. the refinery coke abrasive dust, sieve;
C. by proportioning refinery coke, the modulation agent of carbonaceous aperture structure and binding agent are mixed, stir, knead;
D. through the shaper moulding, dry;
E. charing in charring furnace;
F. in activation furnace, feed the activated media activation.
Delay coking process recited above, processing condition are:
490 ℃~510 ℃ of furnace outlet temperature
415 ℃~420 ℃ of coke drum upper temps
480 ℃~490 ℃ of coke drum temperature of lower
Coke drum pressure 0.2MPa~0.25MPa
Described refinery coke abrasive dust, granularity should be less than 100 orders, preferably less than 160 orders.
0%~6% the water that adds the material weight of kneading in the process of mixing, stir, knead of described refinery coke and modulation agent of carbonaceous aperture and binding agent.
The material moulding 1~5 time on shaper of kneading recited above, molding mass dried 10 minutes~40 minutes.
Described charing operation, 400 ℃~650 ℃ of carbonization temperatures.
Carbonization time is controlled with 20%~45% of the water capacity of charing sample, and preferably 25%~35%.
Described activation procedure, 800 ℃~1000 ℃ of activation temperatures, activated media can be water vapor or carbonic acid gas.Soak time determines by burning the mistake rate, generally burns the mistake rate and is controlled at 60%~70% and gets final product.
Adopt the activated carbon product of method preparation of the present invention, its specification is as follows:
Specific surface area is 500m 2/ g~1200m 2/ g, pore volume 0.45cm 3/ g~0.8cm 3/ g, intensity is 85%~98%, ash content is less than 5%.
The present invention adopts the pre-charing operation of petroleum pitch, promptly uses the delayed coking process of petroleum pitch, makes refinery coke, and after crushed with aperture modulation agent, binding agent and the moulding of water mixing are after step such as charing, activation and make gac.This technology directly adopts existing delay coking process and equipment, make full use of the refinery coke cheap and easy to get of refinery, technology is simple, it is low to pollute, convenient formation, be easy to suitability for industrialized production and avoided pitch in anti-melting process and charing, activation procedure decomposition reaction to take place and produce low-density oil component and objectionable impurities, causes environmental pollution.Owing to contain aperture modulation agent in the prescription, so this gac can be controlled pore size better, can be at different demands, and produce the gac in required aperture, be specially adapted to water conditioning and purifying air, as dyeing and printing sewage processing, electroplating wastewater processing, petrifaction sewage processing, municipal sewage treatment, drink water purifying.
Embodiment 1
With the petrochemical complex mix asphalt is raw material, and it is stable hydrocarbon 44.04% that mix asphalt is formed, aromatic hydrocarbons 25.99%, and colloid 29.03%, bituminous matter 0.74%, density are 0.95478/cm 3, through refinery delay coking process processing unit (plant), hot cracked reaction of mix asphalt and condensation, polyreaction produce C respectively 1-C 4Gaseous fraction and gasoline, diesel oil, wax oil and refinery coke, the delay coking process condition is: 500 ℃ of furnace outlet temperature, 417.5 ℃ of coke drum head temperature, 486.5 ℃ of coke drum bottom temperature, coke drum bottom pressure 0.30MPa, refinery coke character is fugitive constituent 9.2%, ash content 0.42%.
With broken 200 mesh sieves and the coal 3Kg of crossing of refinery coke 7Kg, pitch 4Kg, water 0.7Kg mixes, stirs, kneads.The material of will kneading passes through the shaper moulding secondary of diameter 3.0mm earlier, and then on diameter 1.8mm mould, push post forming, after after the moulding molding mass being dried 30 minutes, carry out charing, carbonization temperature is 500 ℃, carbonization time 7.5 hours, carry out activation procedure then, 920 ℃ of activation temperatures, activated media are water vapor, soak time 5 hours.
The product performance table:
Bulk specific gravity 0.404g/cm 3Ash content 4.14%
Intensity 87% iodine number 917.5mg/g
Methylene blue 165.3mg/g CCL 445.3%
Embodiment 2
With refinery vacuum residuum is raw material, and it consists of stable hydrocarbon 55.92%, aromatic hydrocarbons 25.20%, and colloid 18.47%, bituminous matter are 0.41%, density is 0.9538g/cm 3, through refinery delay coking process processing unit (plant), hot cracked reaction of vacuum residuum and condensation, polyreaction produce C respectively 1-C 4Gas composition and gasoline, diesel oil, wax oil and refinery coke, the delay coking process condition is: 500 ℃ of furnace outlet temperature, 417.5 ℃ of coke drum head temperature, 486.5 ℃ of coke drum bottom temperature, the coke drum bottom pressure is 0.30MPa, and refinery coke character is fugitive constituent 10.5%, ash 0.3%.
With broken 200 mesh sieves of crossing of refinery coke 8Kg, with coal 2Kg, coal tar 3Kg kneads on kneading machine evenly, the material moulding secondary on the shaper of diameter 3.0mm of will kneading, and then on diameter 1.8mm mould, push post forming, after molding mass dries 20 minutes, carry out charing, carbonization temperature is 480 ℃, carry out activation procedure then, activation temperature is 900 ℃, and 4.5 hours time, its product performance are:
Bulk specific gravity 0.442g/cm 3Ash content 4.14%
Methylene blue 128.8mg/g intensity 87.8%
Iodine number 890.4mg/g
Embodiment 3
With refinery vacuum residuum is raw material, and it consists of stable hydrocarbon 56.04%, and aromatic hydrocarbons is 23.24%, and colloid 20.42%, bituminous matter are 0.30%, and density is 0.9557g/cm 3, through refinery delay coking process processing unit (plant), hot cracked reaction of vacuum residuum and condensation, polyreaction produce C respectively 1-C 4Gas composition and gasoline, diesel oil, wax oil and refinery coke, the delay coking process condition is: 500 ℃ of furnace outlet temperature, the coke drum head temperature is 417.5 ℃, the coke drum bottom temperature is 487 ℃, the coke drum bottom pressure is 0.299MPa, refinery coke character is fugitive constituent 9.5%, and ash is 0.39%.
With broken 200 mesh sieves of crossing of refinery coke 8.5kg, with wood charcoal powder 1.5Kg, coal tar 3.0Kg, add water 0.5Kg and on kneading machine, knead evenly, to knead and expect on diameter 4.5mm shaper through three moulding, after molding mass dries 10 minutes, carry out charing, 490 ℃ of carbonization temperatures, activate then, 920 ℃ of activation temperatures, time 4h, its product performance are:
Bulk specific gravity 0.434g/cm 3Ash 2.95%
CCL 466.5% iodine number 992.6mg/g
Yamamoto Methylene Blue ZF suction value 187.6mg/g intensity 88.5%

Claims (12)

1. a petroleum asphalt based active carbon is characterized in that this gac is the refinery coke of being made by petroleum pitch, and modulation agent of carbonaceous aperture structure and binding agent are made, and the weight % content of each component is as follows:
Refinery coke 30%~80%
Carbonaceous aperture structure modulation agent 0%~30%
Binding agent 10%~35%
The main preparation process of this gac comprises pre-charing, kneads, moulding, charing, activation procedure.
2. gac according to claim 1 is characterized in that the used refinery coke of this gac is to be made by petroleum pitch, and each component content is respectively (weight %) in the petroleum pitch:
Stable hydrocarbon 10%~70%
Aromatic hydrocarbon 20%~50%
Colloid 5%~30%
Bituminous matter 0.1%~2.5%
3. gac according to claim 1 is characterized in that the used carbonaceous aperture structure modulation agent of this gac is coal or graphite, starch, charcoal.
4. gac according to claim 1 is characterized in that the used binding agent of this gac is petroleum pitch or coal tar.
5. gac according to claim 4, it is characterized in that used binding agent aromatic hydrocarbons+colloid+bitum total content is 45%~70%, moisture content is less than 5%.
6. the described preparation method of active carbon of claim 1, its feature comprises the steps: successively
A. pre-charing operation is industrial vacuum residuum or cracking of ethylene residual oil, catalytic slurry, the extraction oil of being called with petroleum pitch, and delayed coking process is made refinery coke;
B. the refinery coke abrasive dust, sieve;
C. press proportioning with refinery coke, modulation agent of carbonaceous aperture structure and binding agent mix, stir, knead;
D. through the shaper moulding, dry;
E. charing in charring furnace;
F. in activation furnace, feed the activated media activation.
7. preparation method according to claim 6 is characterized in that the delay coking process condition is:
490 ℃~510 ℃ of furnace outlet temperature
415 ℃~420 ℃ of coke drum upper temps
480 ℃~490 ℃ of coke drum temperature of lower
Coke drum pressure 0.2MPa~0.25MPa
8. preparation method according to claim 6, it is characterized in that the refinery coke abrasive dust after, cross the following sieve of 100 orders.
9. preparation method according to claim 6 is characterized in that refinery coke powder and modulation agent of carbonaceous aperture and binding agent mix, knead in the process, add 0%~6% water.
10. preparation method according to claim 6, the material moulding 1~5 time on shaper that it is characterized in that kneading, molding mass dried 10 minutes~40 minutes.
11. preparation method according to claim 6 is characterized in that carbonization condition is 400 ℃~650 ℃ of carbonization temperatures.
12. preparation method according to claim 6 is characterized in that activation condition is: 800 ℃~1000 ℃ of activation temperatures, activated media is water vapor or carbonic acid gas.
CN97101542A 1997-01-28 1997-01-28 Petroleum asphalt based active carbon and its prepn. method Expired - Fee Related CN1076006C (en)

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Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1076011C (en) * 1998-01-13 2001-12-12 南通碳素厂 Porous carbon material producing process
CN1304283C (en) * 2005-02-22 2007-03-14 东华大学 Prepn process of foamed asphalt carbon material
CN102188954B (en) * 2010-03-03 2013-04-24 中国石油天然气股份有限公司 Activated carbon for adsorbing and removing sulfide in gasoline and preparation method thereof
CN101987921B (en) * 2010-08-18 2011-11-02 中国禾森石化控股有限公司 Natural negative ion composite modified asphalt and preparation method thereof
CN102897761A (en) * 2012-09-26 2013-01-30 南京正森环保科技有限公司 Preparation method of special activated carbon used for carbon canister of automobile or motorcycle
CN103896266A (en) * 2014-04-21 2014-07-02 江苏南凯活性炭有限公司 Method for producing coal and wood mixed solvent recovery active carbon
CN107311170B (en) * 2017-06-26 2019-05-24 中石化炼化工程(集团)股份有限公司 A kind of method and the active carbon preparing active carbon using slurry oil waste residue
CN111841494A (en) * 2020-07-02 2020-10-30 江苏竹溪活性炭有限公司 Active carbon for air purification

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1104175A (en) * 1993-12-21 1995-06-28 中国石油化工总公司石油化工科学研究院 Method for preparation of active carbon
CN1104174A (en) * 1993-12-21 1995-06-28 中国石油化工总公司石油化工科学研究院 Method for preparation of active carbon

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1104175A (en) * 1993-12-21 1995-06-28 中国石油化工总公司石油化工科学研究院 Method for preparation of active carbon
CN1104174A (en) * 1993-12-21 1995-06-28 中国石油化工总公司石油化工科学研究院 Method for preparation of active carbon

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