CN111167408A - Method for preparing adsorption material from oil sludge and application of adsorption material - Google Patents

Method for preparing adsorption material from oil sludge and application of adsorption material Download PDF

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Publication number
CN111167408A
CN111167408A CN202010117914.1A CN202010117914A CN111167408A CN 111167408 A CN111167408 A CN 111167408A CN 202010117914 A CN202010117914 A CN 202010117914A CN 111167408 A CN111167408 A CN 111167408A
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China
Prior art keywords
oil sludge
adsorption material
preparing
oil
sludge
Prior art date
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Pending
Application number
CN202010117914.1A
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Chinese (zh)
Inventor
陈新德
张海荣
彭芬
林木茂
熊莲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xuyi Attapulgite Research & Development Center Of Guangzhou Institute Of Energy Conversion Chinese Academy Of Sciences
Jiangsu Senmao Energy Developments Co ltd
Original Assignee
Xuyi Attapulgite Research & Development Center Of Guangzhou Institute Of Energy Conversion Chinese Academy Of Sciences
Jiangsu Senmao Energy Developments Co ltd
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Application filed by Xuyi Attapulgite Research & Development Center Of Guangzhou Institute Of Energy Conversion Chinese Academy Of Sciences, Jiangsu Senmao Energy Developments Co ltd filed Critical Xuyi Attapulgite Research & Development Center Of Guangzhou Institute Of Energy Conversion Chinese Academy Of Sciences
Priority to CN202010117914.1A priority Critical patent/CN111167408A/en
Publication of CN111167408A publication Critical patent/CN111167408A/en
Pending legal-status Critical Current

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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

Abstract

The invention relates to a method for preparing an adsorbing material by using oil sludge and application thereof, and specifically comprises the following steps: and (2) placing oil sludge residues after the oil-containing sludge is pyrolyzed into an ammonium salt solution to be soaked for a certain time, then filtering, placing a filter cake into a tubular furnace, rapidly heating to 450-650 ℃ under the protection of nitrogen, and carbonizing for 1-6 hours at constant temperature to obtain the carbon adsorption material. According to the invention, impurities such as residual coke and heavy oil in the oil sludge are used as carbon sources to prepare the carbon composite adsorption material, so that the pollution problem of the oil sludge is solved, and the prepared adsorption material is used for adsorbing heavy metals in wastewater.

Description

Method for preparing adsorption material from oil sludge and application of adsorption material
Technical Field
The invention relates to a preparation method of an adsorbing material, in particular to a method for preparing the adsorbing material by taking oil sludge as a raw material and application thereof.
Background
The oily sludge (called oil sludge for short) is one of the main pollutants in the petroleum industry, and the main components of the oily sludge comprise aged crude oil, wax, asphaltene, colloid, solid suspended matters, bacteria, salts, acid gas, corrosion products, a large amount of flocculating agents, corrosion inhibitors, scale inhibitors and the like which are added in the production process. The oil sludge belongs to the strictly controlled hazardous waste in the national hazardous waste list, and can be discharged after harmless treatment. At present, oil sludge is treated by dehydration and pyrolysis mainly in China. Under the conditions of high temperature and oxygen deficiency, light components in the oil sludge are separated from the oil sludge, and simultaneously certain solid waste oil sludge is generated, so that if the solid waste oil sludge is simply buried, not only is the resource waste caused, but also the pollution which is difficult to restore is caused to the environment.
Disclosure of Invention
The invention aims to: the method for preparing the adsorbing material by using the oil sludge and the application thereof are provided, the heavy components and the coke which are remained in the oil sludge are used as carbon sources to prepare the carbon adsorbing material, and the recycling and harmless treatment of the oil sludge are realized.
The invention is realized by adopting the following technical scheme: and (3) placing the oil sludge in an ammonium salt solution for soaking for a certain time, then filtering, placing a filter cake in a tubular furnace, rapidly heating to 450-650 ℃ under the protection of nitrogen, and carbonizing for 1-6 hours at constant temperature to obtain the carbon adsorption material.
Wherein the oil sludge is waste residue generated after dehydration and catalytic pyrolysis of oil sludge.
The ammonium salt solution is one or a mixture of ammonium phosphate and ammonium carbonate, the mass percentage concentration of the ammonium salt solution is 5-30%, and the mass ratio of the ammonium salt solution to the oil sludge is 10-30.
Wherein the temperature rise speed is 10-30 ℃/min.
Wherein the soaking time is 24-72 hours.
Wherein, the adsorption material prepared from the oil sludge is used for adsorbing heavy metals in the wastewater.
Compared with the prior art, the invention has the following advantages:
(1) the carbon adsorption material is prepared by using impurities such as residual coke, heavy oil and the like in the oil sludge as a carbon source, so that the problem of environmental pollution of the oil sludge is solved, and the carbon composite adsorption material with higher added value is prepared, thereby changing waste into valuable.
(2) The ammonium salt is decomposed in the roasting process to generate a large amount of ammonia gas, so that the pore-forming can be performed on the carbon material; the effective regulation and control of the pore diameter of the adsorption material can be realized by regulating and controlling the ammonium salt.
(3) The carbon adsorption material prepared by the invention has simple and reliable preparation process and important economic value and practical significance.
Detailed Description
The technical solution of the invention is further illustrated below with reference to specific examples, which are not to be construed as limiting the technical solution. In practice, the technical personnel according to the invention make improvements and modifications, which still belong to the protection scope of the invention.
Example 1: 500 g of oil sludge residue is placed in 5kg of 5% ammonium phosphate triammonium solution for soaking for 72 h, then filtration is carried out, a filter cake is placed in a tubular furnace, the temperature is raised to 450 ℃ at the speed of 10 ℃/min under the protection of nitrogen, and carbonization is carried out for 6 h at constant temperature, thus obtaining the carbon adsorption material.
The adsorption capacities of the composite material on Pb (II), Cd (II) and Cu (II) are respectively 51, 26 and 29 mg/g.
Example 2: 500 g of oil sludge residue is placed in 8 kg of 30% ammonium carbonate solution by mass fraction to be soaked for 24 h, then the filtration is carried out, a filter cake is placed in a tube furnace, the temperature is raised to 650 ℃ at the speed of 30 ℃/min under the protection of nitrogen, and the constant temperature carbonization is carried out for 1h, thus obtaining the carbon adsorption material.
The adsorption capacities of the composite material to Pb (II), Cd (II) and Cu (II) were 47, 20 and 23 mg/g, respectively.
Example 3: 500 g of oil sludge residue is placed in 15 kg of ammonium dihydrogen phosphate solution with the mass fraction of 15% to be soaked for 48 hours, then the mixture is filtered, a filter cake is placed in a tubular furnace, the temperature is raised to 550 ℃ at the speed of 20 ℃/min under the protection of nitrogen, and the mixture is carbonized at constant temperature for 3 hours to obtain the carbon adsorption material.
The adsorption capacities of the composite material to Pb (II), Cd (II) and Cu (II) were 61, 32 and 26 mg/g, respectively.
The technical solution of the present invention is not limited to the above embodiments, and other embodiments obtained according to the technical solution of the present invention should fall within the protection scope of the present invention.

Claims (6)

1. A method for preparing an adsorbing material by using oil sludge is characterized by comprising the following steps: and (3) placing the oil sludge in an ammonium salt solution for soaking for a certain time, then filtering, placing a filter cake in a tubular furnace, rapidly heating to 450-650 ℃ under the protection of nitrogen, and carbonizing for 1-6 hours at constant temperature to obtain the carbon adsorption material.
2. The method for preparing the adsorbing material from the oil sludge as claimed in claim 1, which is characterized in that: the oil sludge is waste residue generated after dehydration, pyrolysis or catalytic pyrolysis of oil sludge.
3. The method for preparing the adsorbing material from the oil sludge as claimed in claim 1, which is characterized in that: the ammonium salt solution is one or a mixture of ammonium phosphate and ammonium carbonate, the mass percentage concentration of the ammonium salt solution is 5-30%, and the mass ratio of the ammonium salt solution to the oil sludge is 10-30.
4. The method for preparing the adsorbing material from the oil sludge as claimed in claim 1, which is characterized in that: the temperature rise speed is 10-30 ℃/min.
5. The method for preparing the adsorbing material from the oil sludge as claimed in claim 1, which is characterized in that: the soaking time is 24-72 h.
6. The application of the adsorption material prepared from the oil sludge is characterized in that: the adsorption material is used for adsorbing heavy metals in the wastewater.
CN202010117914.1A 2020-02-26 2020-02-26 Method for preparing adsorption material from oil sludge and application of adsorption material Pending CN111167408A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010117914.1A CN111167408A (en) 2020-02-26 2020-02-26 Method for preparing adsorption material from oil sludge and application of adsorption material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010117914.1A CN111167408A (en) 2020-02-26 2020-02-26 Method for preparing adsorption material from oil sludge and application of adsorption material

Publications (1)

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CN111167408A true CN111167408A (en) 2020-05-19

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114589198A (en) * 2022-03-09 2022-06-07 北京科技大学 In-situ stabilizing material for multiple heavy metals in acidic arsenic slag and application method thereof

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CN114589198A (en) * 2022-03-09 2022-06-07 北京科技大学 In-situ stabilizing material for multiple heavy metals in acidic arsenic slag and application method thereof

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