CN101343059A - Method for preparing activated carbon from petroleum coke - Google Patents
Method for preparing activated carbon from petroleum coke Download PDFInfo
- Publication number
- CN101343059A CN101343059A CNA2007101226749A CN200710122674A CN101343059A CN 101343059 A CN101343059 A CN 101343059A CN A2007101226749 A CNA2007101226749 A CN A2007101226749A CN 200710122674 A CN200710122674 A CN 200710122674A CN 101343059 A CN101343059 A CN 101343059A
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- CN
- China
- Prior art keywords
- coke
- hour
- active carbon
- refinery coke
- under
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title abstract description 12
- 239000002006 petroleum coke Substances 0.000 title abstract description 5
- 239000000571 coke Substances 0.000 claims abstract description 25
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000011230 binding agent Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000001125 extrusion Methods 0.000 claims abstract description 3
- 230000004913 activation Effects 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000011280 coal tar Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- 239000011294 coal tar pitch Substances 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 239000011301 petroleum pitch Substances 0.000 claims description 2
- 229920003987 resole Polymers 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 230000003213 activating effect Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 238000010000 carbonizing Methods 0.000 abstract 1
- 239000012778 molding material Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 5
- 229910052740 iodine Inorganic materials 0.000 description 5
- 239000011630 iodine Substances 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000003610 charcoal Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000005242 forging Methods 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 241000024287 Areas Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
A method for preparing active carbon by using petroleum coke as a raw material. Crushing the petroleum coke before calcination to 0.1-2.5 mm, and carrying out pre-oxidation treatment in an oxygen-containing atmosphere to oxidize volatile substances to lose and form pre-oxidized coke with the porosity of 80-300 mg/g. Crushing the pre-oxidized coke until 90% of the pre-oxidized coke passes through a 200-mesh sieve, mixing the pre-oxidized coke with a binder according to the volume ratio of 1.5-10: 1, and then carrying out extrusion forming. Carbonizing the molding material, activating with steam and other gases, and cooling to obtain the product with a specific surface area of 700-1200 m2Per gram of activated carbon.
Description
Technical field
The invention provides a kind of method, belong to field of fine chemical with preparing absorbent charcoal with petroleum coke.
Background technology
Refinery coke is as the byproduct of petrochemical complex, abundant raw material, and the carbon content height, generally 85～95%, and ash low (＜0.5%), be the desirable feedstock of preparation gac, but the refinery coke degree of graphitization want high than other a few class raw materials, relatively is difficult to activation.About being that the report of feedstock production gac adopts chemical activation method more with the refinery coke, wherein based on the activation of alkali metal hydroxides such as KOH, alkali charcoal ratio is generally 3～8: 1.U.S. Pat 4082694 is with the activator KOH thorough mixing of refinery coke and 3 times, under 300-500 ℃ of temperature, dewater and activate in advance, activate under 700～1000 ℃ of temperature, mixture cooling after will activating at last and fully washing make the powdered carbon specific surface area and can reach 2600m again
2/ g; Japan's Northwest coke and chemical company KOH direct activation refinery coke with 3 times of amounts under 800 ℃ of reduced pressure have made specific surface greater than 3000m
2The gac of/g (JP 95-215711), and carried out suitability for industrialized production in 1993; CN 1304788A directly mixes the back high-temperature activation with KOH and refinery coke by 5: 1 mass ratio, and the product specific surface area surpasses 3500m
2/ g.Though the gac of this class methods preparation has the specific surface area of superelevation, complex process, yield is low, and uses the very high KOH raw material of price in a large number, causes product cost very high, and the pollution problem in the production process is also very serious simultaneously.
The gac of superhigh specific surface area is owing to cost an arm and a leg, only a small amount of application is arranged in limited fields such as medicine, electronics, and for the main demand market of gac---other Application Areass widely such as food, chemical industry, environmental protection then generally need low price, specific surface area at 1000～1300m
2The product of/g, therefore studying cheaply, the refinery coke activation method has important value.U.S. Associated Oil Company uses Tripyrophosphoric acid living fossil oil coke down at 900 ℃, prepares specific surface area 500m
2The gac of/g; With the steam activation refinery coke, the iodine sorption value that makes gac is 600mg/g to Japanese Patent JP 74-14395 under 900 ℃; Use steam activation after the levigated refinery coke being allocated into auxiliary material moulding such as coal, the iodine number of gained gac can reach 855mg/g (" novel charcoal material ", 2003, Vol.18 (3)); If in refinery coke, add 5% acidic activator, can bring up to 800～900mg/g (" chemistry of forest product and industry ", 2004, Vol.24 (3)) with the iodine sorption value that makes gac behind the steam activation.But, can only be used for low-end markets such as wastewater treatment because these gac specific surface areas are on the low side.
Summary of the invention
The object of the present invention is to provide a kind of is feedstock production excellent property, process of active carbon with low cost with refinery coke before forging.Technical scheme of the present invention is as follows:
Refinery coke is crushed to 0.1～2.5mm before will forging, and under oxygenous atmosphere, is warming up to 300～550 ℃ with the speed of 5～25 ℃/min, and keeps temperature to carry out pre-oxidation treatment, the volatile substances oxidation is burnt lose, and forms preoxidation Jiao with certain porosity.The preoxidation coke powder is broken to 90% crosses 200 orders (75 μ m), again with binding agent by preoxidation Jiao: the binding agent mass ratio is to mix then extrusion molding at 10～1.5: 1.Moulding mixture earlier 400～700 ℃ of following charings 0.2～3 hour, is activated with the gas activation agent then, and activation temperature is 800～950 ℃, and soak time is 1～48 hour, obtains activated carbon product after the cooling.
Refinery coke at first carried out pre-oxidation treatment before the present invention forged.Pre-oxidation treatment is to carry out in oxygenous volume is 5～30% atmosphere.Oil incipient scorch mistake rate was controlled at 5～40% before the pre-oxidation treatment process was forged, and the iodine sorption value of the burnt porosity of preoxidation is controlled at 80～380mg/g.The time of refinery coke pre-oxidation treatment is between 0.2～8 hour before forging.
Binding agent of the present invention is cellulose family organic compound such as coal tar, coal-tar pitch, petroleum pitch, petroleum residual oil, resol and carboxymethyl cellulose.
Gas mixture that gas activation agent of the present invention is water vapor, water vapor and CO or water vapour and Air mixing gas.
Activation temperature of the present invention is 800～950 ℃, and soak time is 1～48 hour.
The present invention has the following advantages:
1. adopt the oxygen pre-oxidation process, the degree of graphitization of refinery coke is reduced, and form more reactive behavior points, make its easier activation.
2. adopt the oxygen pre-oxidation process, make refinery coke form certain hole,, can improve activation efficiency, improve the product yield for activated gas provides unobstructed passage through preoxidation.
3. pretreatment technology is simple, directly utilizes oxygenous atmosphere to handle, and is low for equipment requirements.
4. the gac density height that makes, ash is less than 0.5%, and specific surface area can reach 700～1200m
2/ g.
Embodiment
Example 1
Refinery coke was crushed to 80～120 orders before Jinzhou petrochemical industry forged, and under air atmosphere, was warming up to 420 ℃ with the speed of 10～20 ℃/min, and pre-oxidation treatment 2 hours is burnt mistake rate 30%, the burnt iodine sorption value 235mg/g of preoxidation.The preoxidation focal sphere is milled to 90% crosses 200 orders,, mix, use the forcing machine moulding then, make the moulding mixture of diameter 2mm with kneader with the mass ratio batching of coal tar by 4: 1.Moulding mixture is used steam activation 24 hours down at 850 ℃ then 650 ℃ of following charings 0.5 hour, obtains gac after the cooling, and specific surface area is 1050m
2/ g.
Claims (3)
1. one kind is the feedstock production process of active carbon with the refinery coke, it is characterized by will forge before refinery coke be crushed to 0.1～2.5mm, be to be warming up to 300～550 ℃ under 5～30% the atmosphere at oxygenous volume, and kept temperature 0.2～8 hour, make the volatile substances oxidation burn the mistake rate and be controlled between 5～40%, form the preoxidation Jiao of hole within 80～300mg/g simultaneously; The preoxidation coke powder is broken to 90% crosses 200 orders, again with binding agent by 1.5～10: 1 weight ratio is mixed, extrusion molding then, charing 0.2～3 hour under 400～700 ℃ temperature earlier, under 800～950 ℃ temperature, activate 1～48 hour then, obtain activated carbon product after the cooling with the gas activation agent.
2. preparation process of active carbon according to claim 1 is characterized in that binding agent is coal tar, coal-tar pitch, petroleum pitch, petroleum residual oil, resol and carboxymethyl cellulose class organic compound.
3. preparation process of active carbon according to claim 1 is characterized in that the gas activation agent is gas mixture or water vapour and the Air mixing gas of water vapor, water vapor and CO.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101226749A CN101343059A (en) | 2007-07-12 | 2007-07-12 | Method for preparing activated carbon from petroleum coke |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101226749A CN101343059A (en) | 2007-07-12 | 2007-07-12 | Method for preparing activated carbon from petroleum coke |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101343059A true CN101343059A (en) | 2009-01-14 |
Family
ID=40245199
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101226749A Pending CN101343059A (en) | 2007-07-12 | 2007-07-12 | Method for preparing activated carbon from petroleum coke |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101343059A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674344A (en) * | 2012-05-22 | 2012-09-19 | 韩钊武 | Method for producing activated carbon by coal tar |
| 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 |
| CN103204501A (en) * | 2012-01-12 | 2013-07-17 | 易高环保能源研究院有限公司 | Method for preparation of activated carbon from carbon-rich residue of high temperature coal tar or coal tar pitch |
| CN103350997A (en) * | 2013-07-04 | 2013-10-16 | 陕西煤业化工技术研究院有限责任公司 | Technique for preparing activated carbon with powdered coal pyrolysis powdered coke |
| CN103979536A (en) * | 2014-05-16 | 2014-08-13 | 宁夏宝塔石化科技实业发展有限公司 | Preparation method of special active carbon for adsorbing dioxin |
| CN107128913A (en) * | 2017-06-22 | 2017-09-05 | 江苏浦士达环保科技股份有限公司 | A kind of preparation method of coconut husk column charcoal |
| CN107640768A (en) * | 2017-11-08 | 2018-01-30 | 山西新华化工有限责任公司 | Rich nitrogen is modified the preparation method of desulfurization sorbing material |
| CN109665522A (en) * | 2017-10-16 | 2019-04-23 | 山东欧铂新材料有限公司 | A kind of hydrophilic graphite oil coke prepares the method and supercapacitor of graphene modified activated carbon |
| CN113353915A (en) * | 2021-07-19 | 2021-09-07 | 中国石油化工股份有限公司 | Mesocarbon microbeads, preparation method thereof, spherical porous activated carbon material and application thereof |
| CN114084936A (en) * | 2021-11-24 | 2022-02-25 | 南京信息工程大学 | Carbon material for degrading sulfonamide antibiotics based on electro-Fenton reaction and preparation method thereof |
| CN117383541A (en) * | 2023-12-11 | 2024-01-12 | 成都万潜科延科技有限公司 | Method for preparing carbon material by using mechanical waste oil, carbon material and application |
-
2007
- 2007-07-12 CN CNA2007101226749A patent/CN101343059A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204501B (en) * | 2012-01-12 | 2016-05-11 | 易高环保能源研究院有限公司 | Prepared the method for active carbon by the rich carbon residue of high temperature coal-tar or coal tar asphalt |
| CN103204501A (en) * | 2012-01-12 | 2013-07-17 | 易高环保能源研究院有限公司 | Method for preparation of activated carbon from carbon-rich residue of high temperature coal tar or coal tar pitch |
| CN102674344A (en) * | 2012-05-22 | 2012-09-19 | 韩钊武 | Method for producing activated carbon by coal tar |
| 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 |
| CN103350997A (en) * | 2013-07-04 | 2013-10-16 | 陕西煤业化工技术研究院有限责任公司 | Technique for preparing activated carbon with powdered coal pyrolysis powdered coke |
| CN103350997B (en) * | 2013-07-04 | 2015-05-27 | 陕西煤业化工技术研究院有限责任公司 | Technique for preparing activated carbon with powdered coal pyrolysis powdered coke |
| CN103979536A (en) * | 2014-05-16 | 2014-08-13 | 宁夏宝塔石化科技实业发展有限公司 | Preparation method of special active carbon for adsorbing dioxin |
| CN107128913A (en) * | 2017-06-22 | 2017-09-05 | 江苏浦士达环保科技股份有限公司 | A kind of preparation method of coconut husk column charcoal |
| CN109665522A (en) * | 2017-10-16 | 2019-04-23 | 山东欧铂新材料有限公司 | A kind of hydrophilic graphite oil coke prepares the method and supercapacitor of graphene modified activated carbon |
| CN107640768A (en) * | 2017-11-08 | 2018-01-30 | 山西新华化工有限责任公司 | Rich nitrogen is modified the preparation method of desulfurization sorbing material |
| CN113353915A (en) * | 2021-07-19 | 2021-09-07 | 中国石油化工股份有限公司 | Mesocarbon microbeads, preparation method thereof, spherical porous activated carbon material and application thereof |
| CN114084936A (en) * | 2021-11-24 | 2022-02-25 | 南京信息工程大学 | Carbon material for degrading sulfonamide antibiotics based on electro-Fenton reaction and preparation method thereof |
| CN114084936B (en) * | 2021-11-24 | 2023-10-27 | 南京信息工程大学 | Carbon material for degrading sulfonamide antibiotics based on electro-Fenton reaction and preparation method thereof |
| CN117383541A (en) * | 2023-12-11 | 2024-01-12 | 成都万潜科延科技有限公司 | Method for preparing carbon material by using mechanical waste oil, carbon material and application |
| CN117383541B (en) * | 2023-12-11 | 2024-02-27 | 成都万潜科延科技有限公司 | Method for preparing carbon material by using mechanical waste oil, carbon material and application |
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Open date: 20090114 |