CN108786726A - A kind of method that tank bottom oil sludge prepares carbon material adsorbing material - Google Patents

A kind of method that tank bottom oil sludge prepares carbon material adsorbing material Download PDF

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Publication number
CN108786726A
CN108786726A CN201810508720.7A CN201810508720A CN108786726A CN 108786726 A CN108786726 A CN 108786726A CN 201810508720 A CN201810508720 A CN 201810508720A CN 108786726 A CN108786726 A CN 108786726A
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China
Prior art keywords
tank
adsorbing
carbon
oil sludge
oil
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CN201810508720.7A
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Chinese (zh)
Inventor
杨慧芬
申康
张鸽
付鹏
李兆峰
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Beijing University of Technology
University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Priority to CN201810508720.7A priority Critical patent/CN108786726A/en
Publication of CN108786726A publication Critical patent/CN108786726A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/10Treatment of sludge; Devices therefor by pyrolysis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/105Phosphorus compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds
    • C02F2101/14Fluorine or fluorine-containing compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/22Chromium or chromium compounds, e.g. chromates
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/40Valorisation of by-products of wastewater, sewage or sludge processing

Abstract

The present invention provides a kind of method that tank bottom oil sludge prepares carbon material adsorbing material, belongs to changing waste into resources and utilizes technical field.This method utilizes tank bottom oil sludge directly as raw material after mixing;After uniformly mixed tank bottom oil sludge is placed in the pyrolysis reactor pyrolysis regular hour under the protection of certain temperature, heating rate and nitrogen atmosphere, it is cooled to room temperature taking-up and obtains original material.Original material is crushed to the final products that certain particle size obtains carbon material adsorbing material.This method can solve the problems, such as that insufficient and traditional sorbing material use cost existing for current petrochemical industry tank bottom oil sludge recycling is high.

Description

A kind of method that tank bottom oil sludge prepares carbon material adsorbing material
Technical field
The present invention relates to changing waste into resources to utilize technical field, particularly relates to a kind of tank bottom oil sludge and prepares carbon material adsorbing material Method.
Background technology
Tank bottom oil sludge is a kind of hazardous solid waste from crude oil drain sump, accumulating tank, slop tank.Petroleum industry exists Due to storing process for a long time in crude oil storage and transport process, heavy components and the entrained with such as paraffin, asphalitine, colloid in oil product A small amount of mechanical admixture, the grains of sand, the inorganic impurities such as soil can due to density contrast natural subsidence, be accumulated in oil storage pot bottom, formed Black but also thick colloid substance layer, referred to as tank bottom oil sludge not only.According to statistics, the crude oil per 90000 cubic metres of storage and transportation, averagely will produce 2000 cubic metres of greasy filth.The yield of China Petroleum about 800,000 tons of tank bottom oil sludges of annual generation, only length celebrating, Shengli Oil Field Just at 100,000 tons or more, oil about slatterns 600,000 tons.Tank bottom oil sludge is different from general oily sludge, wherein nytron Object content is high to account for about 70% (its studies on asphaltene account for 7.8%, paraffin account for 6%, ash content account for 4.8%), remaining water for being about 25% Inorganic matter with 5%, therefore is worth with high resource recycling.Tank bottom oil sludge is usually deposited in the form of water-in-oil emulsion It is being in sticky paste, particle is fine and closely woven, and emulsification is serious, poor fluidity.It is domestic at present that reality is still in the processing of greasy filth and recycling Research and pilot scale stage are tested, still lacks and improves reliable technology, technique, lack Typical model project, domestic large oilfield is for example big The oily sludge disposal technology of the generations such as celebrating, triumph, the Liaohe River and huge port mainly has landfill, thickening, curing process, chemistry to remove Oil, catalytic pyrolysis and building materials utilize, and most oil fields domestic at present use the method for disposal that oily sludge directly fills, though simply It is easy, but the significant wastage of resource is caused, and environmental pollution may be caused.Physico-chemical process for the purpose of recycling crude oil, Suitable for the higher tank bottom oil sludge of oil content, need to add expensive medicament or a large amount of energy of consumption in processing procedure Source, it is also possible to cause the secondary pollutions problem such as waste water, waste residue, utilization need to be further processed.
Currently, carbon material adsorbing material includes mainly that granular activated carbon, active carbon fibre peacekeeping graphite sorbing material etc. are several, Middle granular activated carbon is most typical carbon material adsorbing material.Granular activated carbon is carbon containing by shell, animal skeleton, coal and petroleum coke etc. Raw material not higher than 500 DEG C charing, water flowing steam activations be prepared, be widely used in environmental protection, chemical industry, food processing, The every field such as refined, the military chemistry protection of hydrometallurgy, drug.Not only oil content is high for tank bottom oil sludge, containing paraffin, asphalitine, The heavys carbonaceous component such as colloid is also higher, and low wave is recycled as the raw material for preparing carbon material adsorbing material and simultaneously using tank bottom oil sludge The oil component of hair property, realizes the complete recycling of tank bottom oil sludge, has no any report both at home and abroad.
Invention content
The technical problem to be solved in the present invention is to provide a kind of methods that tank bottom oil sludge prepares carbon material adsorbing material, utilize stone Change industry largely generate hazardous waste --- tank bottom oil sludge prepares carbon material adsorbing material, and oil recovery simultaneously using pyrolytic process Substance, to realize the full utilization of tank bottom oil sludge full constituent, reduce environmental pollution.
It is as follows that the method comprising the steps of:
(1) it is utilized directly as raw material after being sufficiently mixed tank bottom oil sludge uniformly;
(2) by the tank bottom oil sludge being uniformly mixed in step (1) under the protection of certain temperature, heating rate and nitrogen atmosphere After being placed in the pyrolysis reactor pyrolysis regular hour, gained oil gas is recycled, after obtained solid is cooled to room temperature, taking-up obtains Obtain original material;
(3) original material obtained in step (2) is crushed to certain particle size and obtains carbon material adsorbing material.
Wherein, tank bottom oil sludge is that petrochemical industry fortune storage is accumulated in oil storage pot bottom, complicated component, contains nytron in the process Sticky, the dark gum matter of object.
In step (2) pyrolysis temperature be 650~800 DEG C, heating rate be 3~8 DEG C/min, pyrolysis time be 30~ 90min。
Nitrogen flow is 50~200mL/min in step (2).
The granularity of the carbon material adsorbing material obtained in step (3) is less than 1mm.
Element mass content is in the carbon material adsorbing material obtained in step (3):Carbon:30-40%, iron:20-26%, sulphur: 15-20%, aluminium:3-5%, silicon:0.5-3%, calcium:1-6%.The carbon material adsorbing material of acquisition is used for sexavalence in Adsorption water The anion such as chromium, phosphate radical, fluorine.
Hydrocarbons content > 70% in tank bottom oil sludge, studies on asphaltene accounts for 10-15%, colloid accounts for 8-12%, fragrance Hydrocarbon 15-20%, saturated hydrocarbons 45-55%, moisture<25%, inorganic content<5%.
The above-mentioned technical proposal of the present invention has the beneficial effect that:
Carbon material adsorbing material prepares hazardous solid waste-tank bottom oil sludge that raw material is petrochemical industry, system in the present invention Preparation Method is simple, equipment is ripe, and preparation process is not necessarily to add any chemical agent the complete profit, it can be achieved that tank bottom oil sludge full constituent With.This method can solve existing for current petrochemical industry tank bottom oil sludge recycling insufficient and traditional sorbing material use at This high problem.
Description of the drawings
Fig. 1 is that the tank bottom oil sludge of the present invention prepares the method and process flow chart of carbon material adsorbing material;
Fig. 2 is the SEM image of carbon material adsorbing material made from the method for the present invention.
Specific implementation mode
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool Body embodiment is described in detail.
The present invention provides a kind of method that tank bottom oil sludge prepares carbon material adsorbing material.
As shown in Figure 1, substantially steps are as follows for this method:
(1) it is utilized directly as raw material after being sufficiently mixed tank bottom oil sludge uniformly;
(2) by the tank bottom oil sludge being uniformly mixed in step (1) under the protection of certain temperature, heating rate and nitrogen atmosphere After being placed in the pyrolysis reactor pyrolysis regular hour, gained oil gas is recycled, after obtained solid is cooled to room temperature, taking-up obtains Obtain original material;
(3) original material obtained in step (2) is crushed to certain particle size and obtains carbon material adsorbing material.
SEM image by carbon material adsorbing material made from this method is as shown in Figure 2.
It is explained with reference to specific embodiment.
Embodiment 1
Tank bottom oil sludge is sufficiently mixed to the tank bottom oil sludge for uniformly taking 50g uniformly mixed and is put into corundum crucible, is placed in tube furnace Flat-temperature zone is passed through the nitrogen of 100mL/min toward tube furnace, cooling after being warming up to 800 DEG C of heat preservation 60min with the speed of 5 DEG C/min To room temperature, grinding acquisition -1mm carbon material adsorbing materials, in the carbon material adsorbing material, carbon containing 39.55%, iron 25.68%, sulphur 16.86%, aluminium 4.19%, silicon 2.13%, calcium 5.77%.It can be 39.96mg/g to the adsorbance of Cr VI in water.
Embodiment 2
Tank bottom oil sludge is sufficiently mixed to the tank bottom oil sludge for uniformly taking 50g uniformly mixed and is put into corundum crucible, is placed in tube furnace Flat-temperature zone is passed through the nitrogen of 100mL/min toward tube furnace, cooling after being warming up to 750 DEG C of heat preservation 60min with the speed of 3 DEG C/min To room temperature, grinding acquisition -1mm carbon material adsorbing materials, in the carbon material adsorbing material, carbon containing 37.41%, iron 25.32%, sulphur 18.43%, aluminium 4.06%, silicon 2.70%, calcium 6.00%.It can be 37.37mg/g to the adsorbance of Cr VI in water.
Embodiment 3
Tank bottom oil sludge is sufficiently mixed to the tank bottom oil sludge for uniformly taking 50g uniformly mixed and is put into corundum crucible, is placed in tube furnace Flat-temperature zone is passed through the nitrogen of 200mL/min toward tube furnace, cooling after being warming up to 750 DEG C of heat preservation 60min with the speed of 5 DEG C/min To room temperature, grinding acquisition -1mm carbon material adsorbing materials, in the carbon material adsorbing material, carbon containing 39.23%, iron 25.23%, sulphur 16.11%, aluminium 4.21%, silicon 2.06%, calcium 5.23%.It can be 38.22mg/g to the adsorbance of Cr VI in water.
Embodiment 4
Tank bottom oil sludge is sufficiently mixed to the tank bottom oil sludge for uniformly taking 50g uniformly mixed and is put into corundum crucible, is placed in tube furnace Flat-temperature zone is passed through the nitrogen of 100mL/min toward tube furnace, cooling after being warming up to 750 DEG C of heat preservation 75min with the speed of 5 DEG C/min To room temperature, grinding acquisition -1mm carbon material adsorbing materials, in the carbon material adsorbing material, carbon containing 39.54%, iron 25.35%, sulphur 18.87%, aluminium 4.21%, silicon 2.16%, calcium 5.92%.It can be 41.83mg/g to the adsorbance of Cr VI in water.
Embodiment 5
Tank bottom oil sludge is sufficiently mixed to the tank bottom oil sludge for uniformly taking 50g uniformly mixed and is put into corundum crucible, is placed in tube furnace Flat-temperature zone is passed through the nitrogen of 100mL/min toward tube furnace, cooling after being warming up to 750 DEG C of heat preservation 75min with the speed of 5 DEG C/min To room temperature, grinding acquisition -1mm carbon material adsorbing materials, in the carbon material adsorbing material, carbon containing 39.54%, iron 25.35%, sulphur 18.87%, aluminium 4.21%, silicon 2.16%, calcium 5.92%.It can be 19.95mg/g to the adsorbance of phosphate radical in water.
Embodiment 6
Tank bottom oil sludge is sufficiently mixed to the tank bottom oil sludge for uniformly taking 50g uniformly mixed and is put into corundum crucible, is placed in tube furnace Flat-temperature zone is passed through the nitrogen of 100mL/min toward tube furnace, cooling after being warming up to 750 DEG C of heat preservation 75min with the speed of 5 DEG C/min To room temperature, grinding acquisition -1mm carbon material adsorbing materials, in the carbon material adsorbing material, carbon containing 39.54%, iron 25.35%, sulphur 18.87%, aluminium 4.21%, silicon 2.16%, calcium 5.92%.It can be 35.53mg/g to the adsorbance of fluorine in water.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (8)

1. a kind of method that tank bottom oil sludge prepares carbon material adsorbing material, it is characterised in that:Including steps are as follows:
(1) it is utilized directly as raw material after being sufficiently mixed tank bottom oil sludge uniformly;
(2) tank bottom oil sludge being uniformly mixed in step (1) is placed under the protection of certain temperature, heating rate and nitrogen atmosphere After pyrolysis reactor is pyrolyzed the regular hour, gained oil gas is recycled, after obtained solid is cooled to room temperature, takes out and obtains just Beginning material;
(3) original material obtained in step (2) is crushed to certain particle size and obtains carbon material adsorbing material.
2. the method that tank bottom oil sludge according to claim 1 prepares carbon material adsorbing material, it is characterised in that:The tank bottom oil Mud is sticky, the dark gum that petrochemical industry fortune storage is accumulated in oil storage pot bottom, complicated component, hydrocarbon-containiproducts in the process Matter.
3. the method that tank bottom oil sludge according to claim 1 prepares carbon material adsorbing material, it is characterised in that:The step (2) pyrolysis temperature is 650~800 DEG C in, and heating rate is 3~8 DEG C/min, and pyrolysis time is 30~90min.
4. the method that tank bottom oil sludge according to claim 1 prepares carbon material adsorbing material, it is characterised in that:The step (2) nitrogen flow is 50~200mL/min in.
5. the method that tank bottom oil sludge according to claim 1 prepares carbon material adsorbing material, it is characterised in that:The step (3) granularity of the carbon material adsorbing material obtained in is less than 1mm.
6. the method that tank bottom oil sludge according to claim 1 prepares carbon material adsorbing material, it is characterised in that:The step (3) carbon material adsorbing material obtained in is for Cr VI, phosphate radical, fluorine anion in Adsorption water.
7. the method that tank bottom oil sludge according to claim 1 prepares carbon material adsorbing material, it is characterised in that:The tank bottom oil Hydrocarbons content > 70% in mud, studies on asphaltene accounts for 10-15%, colloid accounts for 8-12%, aromatic hydrocarbon accounts for 15-20%, full 45-55%, moisture are accounted for hydrocarbon<25%, inorganic content<5%.
8. the method that tank bottom oil sludge according to claim 1 prepares carbon material adsorbing material, it is characterised in that:The step (3) element mass content is in the carbon material adsorbing material obtained in:Carbon:30-40%, iron:20-26%, sulphur:15-20%, aluminium: 3-5%, silicon:0.5-3%, calcium:1-6%.
CN201810508720.7A 2018-05-24 2018-05-24 A kind of method that tank bottom oil sludge prepares carbon material adsorbing material Pending CN108786726A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111039345A (en) * 2020-01-06 2020-04-21 北京科技大学 High-added-value resource utilization method of oil sludge pyrolysis slag

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Publication number Priority date Publication date Assignee Title
CN101759339A (en) * 2010-01-11 2010-06-30 清华大学 Reclamation treatment method of oil field tank bottom oil sludge
CN102294217A (en) * 2011-06-23 2011-12-28 中国石油天然气集团公司 Method for preparing new oil-extraction wastewater adsorbent by using pyrolysis residues of oil sludge
CN102849905A (en) * 2012-03-22 2013-01-02 中国石油天然气股份有限公司 Experimental method of oil-containing sludge heat treatment
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