CN107285309A - A kind of oily sludge and the biomass combined method for preparing multistage mesoporous activated carbon - Google Patents
A kind of oily sludge and the biomass combined method for preparing multistage mesoporous activated carbon Download PDFInfo
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/12—Surface area
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- C01P2006/14—Pore volume
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- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The invention discloses a kind of oily sludge and the biomass combined method for preparing multistage mesoporous activated carbon, comprise the following steps：By oily sludge centrifuging and taking upper oil phase, it is put into after being mixed with biological particles in tube furnace, is warming up to 350 450 DEG C with 25 DEG C/min under inert atmosphere protection and is incubated 90 120min, be cooled to room temperature and complete carbonisation；Then solid is uniformly mixed with KOH, 800 850 DEG C of 60 90min of insulation is warming up under inert atmosphere protection, natural cooling completes activating process；The grinding of gained solid washing and drying is obtained into the multistage mesoporous activated carbon.The activated carbon specific surface area prepared is more than 1800m2/ g, average pore size 3nm or so.The present invention using biomass and high viscosity, complicated component oily sludge as raw material, with raw material sources are wide, cost is low, equipment is simple, pollution-free, the advantage that the accessory substance in preparation process can be recycled.
Description
Technical field
The present invention relates to biological in the poisonous and harmful solid waste of petroleum chemical industry oily sludge and agricultural production process
Matter utilization of waste as resource technical field, more particularly to a kind of oily sludge and the multistage mesoporous activated carbon of biomass combined preparation
Method.
Background technology
Oily sludge be produced during crude oil exploration, exploitation, transport, storage, clear tank, refining etc. a kind of water, oil,
The thick solid discarded object that slag is highly emulsified.Oily sludge complicated component, containing substantial oil, asphalitine, wax, moisture,
Solid particle and various medicaments, with difficult degradation, it is poisonous, harmful the features such as, not disposable and pollution environment belongs to national danger
Hazardous waste classification HW08 in dangerous waste register.Generally, oily sludge contains 30-50% water, 10-12% solid particle and
30-50% oil, and oil phase is made up of saturated hydrocarbons, aromatic hydrocarbon, resin and asphalt.The presence of resin and asphalt is promoted
The stability of emulsion in oily sludge, considerably increases the intractability of oily sludge.At present, burning method be oily sludge without
One of evilization processing method, but the problem of exist that cost is high, be also easy to produce secondary pollution.And recycling processing method is mainly wrapped
Include：Mechanically decoupled, chemical extraction and thermal conversion process, but be due to the high viscosity and high toxicity of oily sludge, there is also effect
The deficiencies such as undesirable, complex operation.
Biomass is as a kind of agricultural wastes, and with wide material sources, that yield is high, cheap, growth cycle is short etc. is excellent
Gesture, and compared with feed coal, biomass no adhesion, without the broken specially treated such as glutinous.China is as a large agricultural country, often
Biomass such as stalk, rice husk, the corncob Isoquant in year are very big.Traditional biomass method of disposal, such as burning method is easily caused
The wasting of resources and environmental pollution.The resource utilization method of current biomass is mainly thermal conversion process, but there is also production
The problems such as article matter is not high, equipment is complicated.
Activated carbon is that a kind of specific surface area is high, and surface has the material of loose structure.Because it has unique absorption table
Face architectural characteristic and surface chemistry, activated carbon have stronger absorption property and catalytic performance, and activated carbon preparing raw material is filled
Sufficient and safe, acid and alkali-resistance, easily heat-resisting, water insoluble and organic solvent, regeneration, are a kind of environmentally friendly adsorbents.Mesh
Before, activated carbon is widely used to the every field such as chemical industry, environmental protection, food processing, metallurgy, refined, the military chemistry protection of medicine.
Active Carbon Materials are by the amorphous carbon obtained by working process, specific surface area as raw materials such as coal, coconut husk, shell, wood chips
Typically smaller than 1100m2/ g and many based on mesoporous.And the activated carbon for being used for specific use is by expensive asphalitine and macromolecule
Polymeric material is made, and specific surface area is more than 2000m2/g.Multistage mesoporous activated carbon is referred in activated carbon while being distributed with substantial amounts of
Mesoporous and micropore, has very high adsorption capacity to the ion and organic pollutant in gas molecule and liquid phase.
Belong to the money of dangerous solid waste with the multistage mesoporous activated carbon technology of preparing of oily sludge and biomass compound
Source utilizes field.The present invention is with the oily sludge produced in crude oil production process and the biomass produced in agricultural production
Compound is object, and according to the principle of " innoxious, minimizing, recycling ", for oily sludge, difficult, asphalitine contains in itself
Amount is high, the features such as yield of biomass is big, and research oily sludge and biomass compound prepare multi-stage porous activated carbon technology.For oil-containing
Sludge and the recycling and its industrialized production of biomass provide new approaches and new method, have important practical significance.
Chinese patent CN201611234477.1 discloses a kind of preparation method of the common coking activated carbon of biomass-residual oil,
Biomass and residual oil are subjected to co carbonization reaction under inert gas shielding, common coking is obtained；Common coking is carried out successively hydrophilic
Property pretreatment and except ash content pretreatment, obtain it is pretreated altogether coking；, will be pretreated under the conditions of inert gas shielding
Coking roasting, obtains bio-based Carbon Materials altogether；Under inert gas shielding, bio-based carbon material and activator activate instead
Should, obtaining biomass-residual oil, coking activated carbon has high-specific surface area, high pore volume characteristic altogether.
The content of the invention
It is oil-containing it is an object of the invention to a kind of oily sludge and the biomass combined method for preparing multistage mesoporous activated carbon
The recycling of sludge and biomass castoff provides a kind of new approaches.The advantage of the invention is that：Cost is low, easy to operate,
The simple less investment of pollution-free, equipment, and accessory substance in preparation process can recycling, can fully recycle storage
Transport each component of greasy filth and biomass.
In order to achieve the above object, the technical solution adopted by the present invention includes：
A kind of method of oily sludge and the multistage mesoporous activated carbon of biomass combined preparation, the specific surface area of the activated carbon exists
1800m2/ more than g, pore-size distribution is mainly between 0.5-4nm, and average pore size is more than 1.5cm in 3nm or so, pore volume3/g；Bag
Include following steps：
Step (1), oily sludge is centrifuged after, remove middle level moisture and bottom solid slag, obtain upper strata oil
Phase product；
Step (2), by biomass crushing grinding, obtain biological particles；
Step (3), by the biological particles obtained by the oil-phase product obtained by step (1) and step (2) with mass ratio 1：
(0.2-1) uniformly after mixing, is put into corundum crucible, 350-450 DEG C is warming up to simultaneously with 2-5 DEG C/min under inert atmosphere protection
90-120min is incubated, naturally cools to and blocks of solid is obtained after room temperature, grind to form particle；
Step (4), step (3) obtained to be put into corundum crucible after solid particle is uniformly mixed with KOH powder, in inertia
800-850 DEG C is warming up under atmosphere protection, 60-90min is incubated, naturally cools to room temperature, after taking-up with deionized water rinsing extremely
Filtrate obtains the multistage mesoporous activated carbon in neutrality, drying and grinding.
Described oily sludge is a kind of high viscosity, the black emulsus of complicated component that produce in crude oil production process
Thing.
Described biomass be agricultural production process in produce such as stalk, rice husk, solid waste.
Parameter of noncentricity described in step (1) is：3000-4000rpm, centrifuges 10-20min, and process temperature is 15-20 DEG C.
Biological particles described in step (2) are 60-80 mesh or so.
Abrasive grains size described in step (3) is 1.5-2mm
The mixing quality ratio of step (4) solid particle and KOH powder is 1：(3-5).
Oily sludge of the present invention has advantages below with the biomass combined method for preparing multistage mesoporous activated carbon：
1. preparation technology is simple：Centrifuged by oily sludge, biomass is crushed, raw material is mixed, is carbonized, activated, washing, doing
The serial of methods such as dry, grinding, handle oily sludge and biomass, prepare multistage mesoporous activated carbon, preparation technology
Simply, device is easy to get, and operating procedure is few, and feasibility is high；
2. raw material and additive are easy to get：The danger for preparing required oily sludge to produce in crude oil production process
Solid waste；Biomass needed for preparing is the solid waste produced in agricultural production process, and yield is big；In preparation process
Required additive is easy to get；
3. raw material makes full use of：Produce that oil product viscosity is low, molecule in oily sludge and biomass compound carbonisation
Amount is small, and branded oil Product recycling can be used as after processing.
4. the multistage mesoporous activated carbon quality prepared is high：Specific surface area is not less than 1800m2/ g, pore-size distribution is mainly in 0.5-
Between 4nm, average pore size is more than 1.5cm in 3nm or so, pore volume3/g。
Brief description of the drawings
Fig. 1 is oily sludge of the present invention and the biomass combined method flow diagram for preparing multistage mesoporous activated carbon.
Fig. 2 is the scanning electron microscope (SEM) photograph of the gained activated carbon of the embodiment of the present invention 1.
Fig. 3 is N2 adsorption-desorption isotherm figure of the gained activated carbon of the embodiment of the present invention 1.
Fig. 4 is the graph of pore diameter distribution of the gained activated carbon of the embodiment of the present invention 1.
Embodiment
Below, the present invention will be further illustrated with embodiment, but any one being not limited in following examples.Fig. 1 is
Oily sludge of the present invention and the biomass combined method flow diagram for preparing multistage mesoporous activated carbon.
Embodiment 1
Oily sludge using asphalitine mass content as 6% as raw material, at 20 DEG C by 3000rpm, 10min from
Bottom solid particle and moisture are removed after heart processing, upper oil phase is taken.Using rice husk as biomass material, after crushing grinding
Obtain the rice husk particle of 60-80 mesh.By upper oil phase and rice husk particle with mass ratio 1：0.25 uniform mixing.Mixture is put into
Heat carbonization in corundum crucible by atmosphere of nitrogen in tube furnace, heating condition is 4 DEG C/min, be warming up to after 400 DEG C and be incubated
120min, naturally cools to and solid product is obtained after room temperature.Solid product is ground to 2mm or so solid particle, and and KOH
Powder is with mass ratio 1：It is put into corundum crucible, is placed in heat-activated in tube furnace, activation process with nitrogen after 4 uniform mixing
Gas is protective atmosphere, and heating-up temperature is 800 DEG C, and room temperature is naturally cooled to after insulation 60min.Obtained product passes through deionized water
Rinse after being in neutral to filtrate, drying grinding obtains the multistage mesoporous activated carbon, and activated carbon ESEM is as shown in Figure 2.It is made
Standby activated carbon specific surface area is 1849m2/ g, pore volume is 1.58cm3/ g, prepared activated carbon is in relative pressure as shown in Figure 3
Power is significantly increased less than the adsorbance between 0.1 and 0.1-0.9, is illustrated in activated carbon while there is micropore and mesoporous.
Activated carbon pore size is distributed between 0.8-4.1nm as shown in Figure 4, and average pore size is 2.81nm, the suction to water body Methylene Blue
Attached amount is 931mg/g.
Embodiment 2
Oily sludge using asphalitine mass content as 11% is as raw material, by 3500rpm, 10min at 20 DEG C
Bottom solid particle and moisture are removed after centrifugal treating, upper oil phase is taken.Using rice husk as biomass material, by crushing grinding
The rice husk particle of 60-80 mesh is obtained afterwards.By upper oil phase and rice husk particle with mass ratio 1：0.25 uniform mixing.Mixture is put
Enter and heat carbonization in corundum crucible by atmosphere of nitrogen in tube furnace, heating condition is 4 DEG C/min, be warming up to after 400 DEG C and protect
Warm 120min, naturally cools to and solid product is obtained after room temperature.Solid product is ground to 2mm or so solid particle, and with
KOH powder is with mass ratio 1：It is put into corundum crucible, is placed in heat-activated in tube furnace, activation process after 4 uniform mixing
Using nitrogen as protective atmosphere, heating-up temperature is 800 DEG C, and room temperature is naturally cooled to after insulation 60min.Obtained product through the past from
Sub- water is rinsed to filtrate in after neutral, and drying grinding obtains the multistage mesoporous activated carbon.Prepared activated carbon specific surface area is
2142m2/ g, pore volume is 1.85cm3/ g, average pore size is 3.04nm, and the adsorbance to water body Methylene Blue is 1038mg/
g。
Embodiment 3
Oily sludge using asphalitine mass content as 11% is as raw material, by 4000rpm, 15min at 20 DEG C
Bottom solid particle and moisture are removed after centrifugal treating, upper oil phase is taken.Using rice husk as biomass material, by crushing grinding
The rice husk particle of 60-80 mesh is obtained afterwards.By upper oil phase and rice husk particle with mass ratio 1：1 uniform mixing.Mixture is put into
Heat carbonization in corundum crucible by atmosphere of nitrogen in tube furnace, heating condition is 4 DEG C/min, be warming up to after 400 DEG C and be incubated
120min, naturally cools to and solid product is obtained after room temperature.Solid product is ground to 2mm or so solid particle, and and KOH
Powder is with mass ratio 1：It is put into corundum crucible, is placed in heat-activated in tube furnace, activation process with nitrogen after 4 uniform mixing
Gas is protective atmosphere, and heating-up temperature is 800 DEG C, and room temperature is naturally cooled to after insulation 60min.Obtained product passes through deionized water
Rinse after being in neutral to filtrate, drying grinding obtains the multistage mesoporous activated carbon.Prepared activated carbon specific surface area is
1976m2/ g, pore volume is 1.68cm3/ g, average pore size is 2.74nm, and the adsorbance to water body Methylene Blue is 891mg/g.
Embodiment 4
Oily sludge using asphalitine mass content as 11% is as raw material, by 3000rpm, 15min at 20 DEG C
Bottom solid particle and moisture are removed after centrifugal treating, upper oil phase is taken.Using rice husk as biomass material, by crushing grinding
The rice husk particle of 60-80 mesh is obtained afterwards.By upper oil phase and rice husk particle with mass ratio 1：0.3 uniform mixing.Mixture is put
Enter and heat carbonization in corundum crucible by atmosphere of nitrogen in tube furnace, heating condition is 4 DEG C/min, be warming up to after 400 DEG C and protect
Warm 120min, naturally cools to and solid product is obtained after room temperature.Solid product is ground to 2mm or so solid particle, and with
KOH powder is with mass ratio 1：It is put into corundum crucible, is placed in heat-activated in tube furnace, activation process after 4 uniform mixing
Using nitrogen as protective atmosphere, heating-up temperature is 800 DEG C, and room temperature is naturally cooled to after insulation 60min.Obtained product through the past from
Sub- water is rinsed to filtrate in after neutral, and drying grinding obtains the multistage mesoporous activated carbon.Prepared activated carbon specific surface area is
2254m2/ g, pore volume is 1.87cm3/ g, average pore size is 3.12nm, and the adsorbance to water body Methylene Blue is 1044mg/
g。
Embodiment 5
Oily sludge using asphalitine mass content as 6% as raw material, at 15 DEG C by 4000rpm, 20min from
Bottom solid particle and moisture are removed after heart processing, upper oil phase is taken.Using rice husk as biomass material, after crushing grinding
Obtain the rice husk particle of 60-80 mesh.By upper oil phase and rice husk particle with mass ratio 1：0.2 uniform mixing.Mixture is put into
Heat carbonization in corundum crucible by atmosphere of nitrogen in tube furnace, heating condition is 4 DEG C/min, be warming up to after 400 DEG C and be incubated
120min, naturally cools to and solid product is obtained after room temperature.Solid product is ground to 2mm or so solid particle, and and KOH
Powder is with mass ratio 1：It is put into corundum crucible, is placed in heat-activated in tube furnace, activation process with nitrogen after 4 uniform mixing
Gas is protective atmosphere, and heating-up temperature is 800 DEG C, and room temperature is naturally cooled to after insulation 60min.Obtained product passes through deionized water
Rinse after being in neutral to filtrate, drying grinding obtains the multistage mesoporous activated carbon.Prepared activated carbon specific surface area is
1985m2/ g, pore volume is 1.61cm3/ g, average pore size is 2.95nm, and the adsorbance to water body Methylene Blue is 895mg/g.
Embodiment 6
Oily sludge using asphalitine mass content as 6% as raw material, at 20 DEG C by 4000rpm, 10min from
Bottom solid particle and moisture are removed after heart processing, upper oil phase is taken.Using rice husk as biomass material, after crushing grinding
Obtain the rice husk particle of 60-80 mesh.By upper oil phase and rice husk particle with mass ratio 1：0.2 uniform mixing.Mixture is put into
Heat carbonization in corundum crucible by atmosphere of nitrogen in tube furnace, heating condition is 2 DEG C/min, be warming up to after 350 DEG C and be incubated
120min, naturally cools to and solid product is obtained after room temperature.Solid product is ground to 2mm or so solid particle, and and KOH
Powder is with mass ratio 1：It is put into corundum crucible, is placed in heat-activated in tube furnace, activation process with nitrogen after 3 uniform mixing
Gas is protective atmosphere, and heating-up temperature is 850 DEG C, and room temperature is naturally cooled to after insulation 90min.Obtained product passes through deionized water
Rinse after being in neutral to filtrate, drying grinding obtains the multistage mesoporous activated carbon.Prepared activated carbon specific surface area is
1885m2/ g, pore volume is 1.78cm3/ g, average pore size is 2.90nm, and the adsorbance to water body Methylene Blue is 845mg/g.
Embodiment 7
Oily sludge using asphalitine mass content as 11% is as raw material, by 4000rpm, 10min at 17 DEG C
Bottom solid particle and moisture are removed after centrifugal treating, upper oil phase is taken.Using rice husk as biomass material, by crushing grinding
The rice husk particle of 60-80 mesh is obtained afterwards.By upper oil phase and rice husk particle with mass ratio 1：0.5 uniform mixing.Mixture is put
Enter and heat carbonization in corundum crucible by atmosphere of nitrogen in tube furnace, heating condition is 5 DEG C/min, be warming up to after 450 DEG C and protect
Warm 90min, naturally cools to and solid product is obtained after room temperature.Solid product is ground to 2mm or so solid particle, and with
KOH powder is with mass ratio 1：It is put into corundum crucible, is placed in heat-activated in tube furnace, activation process after 5 uniform mixing
Using nitrogen as protective atmosphere, heating-up temperature is 820 DEG C, and room temperature is naturally cooled to after insulation 70min.Obtained product through the past from
Sub- water is rinsed to filtrate in after neutral, and drying grinding obtains the multistage mesoporous activated carbon.Prepared activated carbon specific surface area is
2112m2/ g, pore volume is 1.83cm3/ g, average pore size is 3.08nm, and the adsorbance to water body Methylene Blue is 1103mg/
g。
Claims (8)
1. a kind of oily sludge exists with the biomass combined method for preparing multistage mesoporous activated carbon, the specific surface area of the activated carbon
1800m2/ more than g, pore-size distribution is mainly between 0.5-4nm, and average pore size is more than 1.5cm in 3nm or so, pore volume3/g；Its
It is characterised by that this method comprises the following steps：
Step (1), oily sludge is centrifuged after, remove middle level moisture and bottom solid slag, obtain upper oil phase production
Thing；
Step (2), by biomass crushing grinding, obtain biological particles；
Step (3), by obtained by the oil-phase product obtained by step (1) and step (2) biological particles uniformly mixing after, be put into just
In beautiful crucible, it is warming up to 350-450 DEG C with 2-5 DEG C/min under inert atmosphere protection and is incubated 90-120min, naturally cool to
Blocks of solid is obtained after room temperature, particle is ground to form；
Step (4), step (3) obtained to be put into corundum crucible after solid particle is uniformly mixed with KOH powder, in inert atmosphere
800-850 DEG C is warming up under protection, 60-90min is incubated, room temperature is naturally cooled to, with deionized water rinsing to filtrate after taking-up
In neutrality, drying and grinding obtains the multistage mesoporous activated carbon.
2. a kind of oily sludge as claimed in claim 1 and the biomass combined method for preparing multistage mesoporous activated carbon, its feature
It is a kind of high viscosity, the black milk of complicated component produced in crude oil production process to be described oily sludge.
3. a kind of oily sludge as claimed in claim 1 and the biomass combined method for preparing multistage mesoporous activated carbon, its feature
The solid waste for being described biomass to produce in agricultural production process.
4. a kind of oily sludge as claimed in claim 1 and the biomass combined method for preparing multistage mesoporous activated carbon, its feature
It is that the parameter of noncentricity described in step (1) is：3000-4000rpm, centrifuges 10-20min, and process temperature is 15-20 DEG C.
5. a kind of oily sludge as claimed in claim 1 and the biomass combined method for preparing multistage mesoporous activated carbon, its feature
It is 60-80 mesh or so to be the biological particles described in step (2).
6. a kind of oily sludge as claimed in claim 1 and the biomass combined method for preparing multistage mesoporous activated carbon, its feature
It is 1.5-2m to be the abrasive grains size described in step (3).
7. a kind of oily sludge as claimed in claim 1 and the biomass combined method for preparing multistage mesoporous activated carbon, its feature
The mass ratio for being the biological particles obtained by the oil-phase product and step (2) obtained by step (3) step (1) is 1：(0.2-1).
8. a kind of oily sludge as claimed in claim 1 and the biomass combined method for preparing multistage mesoporous activated carbon, its feature
The mixing quality ratio for being step (4) solid particle and KOH powder is 1：(3-5).
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| CN109174063A (en) * | 2018-10-17 | 2019-01-11 | 肇庆市珈旺环境技术研究院 | A kind of sludge base adsorbent and preparation method thereof |
| CN110479209A (en) * | 2019-09-03 | 2019-11-22 | 邓晖 | A kind of natural minerals/absorbent charcoal composite material and preparation method thereof |
| CN111533126A (en) * | 2020-05-22 | 2020-08-14 | 东华大学 | Preparation method of high-compressive-strength high-porosity formed sludge activated carbon |
| CN112408390A (en) * | 2020-11-20 | 2021-02-26 | 西北化工研究院有限公司 | Method for preparing activated carbon adsorbent from kerosene co-refining residues |
| CN113772671A (en) * | 2021-10-27 | 2021-12-10 | 西安交通大学 | Improved coal-based activated carbon and preparation method and application thereof |
| CN114073932A (en) * | 2020-08-14 | 2022-02-22 | 中国石油天然气集团有限公司 | Oil product adsorbing material and preparation method thereof |
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| CN108773840A (en) * | 2018-06-07 | 2018-11-09 | 广西壮族自治区环境保护科学研究院 | A kind of method that destructive distillation oily sludge prepares charcoal |
| CN109174063A (en) * | 2018-10-17 | 2019-01-11 | 肇庆市珈旺环境技术研究院 | A kind of sludge base adsorbent and preparation method thereof |
| CN110479209A (en) * | 2019-09-03 | 2019-11-22 | 邓晖 | A kind of natural minerals/absorbent charcoal composite material and preparation method thereof |
| CN111533126A (en) * | 2020-05-22 | 2020-08-14 | 东华大学 | Preparation method of high-compressive-strength high-porosity formed sludge activated carbon |
| CN114073932A (en) * | 2020-08-14 | 2022-02-22 | 中国石油天然气集团有限公司 | Oil product adsorbing material and preparation method thereof |
| CN114073932B (en) * | 2020-08-14 | 2024-04-30 | 中国石油天然气集团有限公司 | Oil adsorption material and preparation method thereof |
| CN112408390A (en) * | 2020-11-20 | 2021-02-26 | 西北化工研究院有限公司 | Method for preparing activated carbon adsorbent from kerosene co-refining residues |
| CN113772671A (en) * | 2021-10-27 | 2021-12-10 | 西安交通大学 | Improved coal-based activated carbon and preparation method and application thereof |
| CN113772671B (en) * | 2021-10-27 | 2024-03-29 | 西安交通大学 | Improved coal-based activated carbon and preparation method and application thereof |
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