CN115532233B - Asphaltene-based adsorption material, and preparation method and application thereof - Google Patents
Asphaltene-based adsorption material, and preparation method and application thereof Download PDFInfo
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- CN115532233B CN115532233B CN202110723572.2A CN202110723572A CN115532233B CN 115532233 B CN115532233 B CN 115532233B CN 202110723572 A CN202110723572 A CN 202110723572A CN 115532233 B CN115532233 B CN 115532233B
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000000203 mixture Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000002351 wastewater Substances 0.000 claims abstract description 26
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000002244 precipitate Substances 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 12
- 239000012190 activator Substances 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000003463 adsorbent Substances 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims description 5
- 239000010426 asphalt Substances 0.000 claims description 4
- 239000000295 fuel oil Substances 0.000 claims description 4
- KWHDXJHBFYQOTK-UHFFFAOYSA-N heptane;toluene Chemical compound CCCCCCC.CC1=CC=CC=C1 KWHDXJHBFYQOTK-UHFFFAOYSA-N 0.000 claims description 3
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 3
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 3
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 4
- 231100000719 pollutant Toxicity 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 238000011282 treatment Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000010865 sewage Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000003027 oil sand Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 235000013162 Cocos nucifera Nutrition 0.000 description 2
- 244000060011 Cocos nucifera Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- -1 vacuum residuum Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/365—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds from petrochemical industry (e.g. refineries)
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Civil Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Structural Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses an asphaltene-based adsorption material, and a preparation method and application thereof. The method comprises the following steps: (a) Mixing asphaltenes with toluene to obtain a first mixture, and mixing a stripping agent with toluene to obtain a second mixture; (b) Uniformly mixing the first mixture and the second mixture obtained in the step (a), and then standing and filtering to obtain a precipitate; (c) Washing and drying the precipitate obtained in the step (b), and then mixing with chloroform to obtain a third mixture; (d) Extracting the third mixture obtained in step (c) with an activator solution; (e) Mixing the material obtained after the extraction in the step (d) with polyethylene glycol, extruding, forming and post-treating to obtain the asphaltene-based adsorption material. The asphaltene-based adsorption material is used for treating petrochemical wastewater, can realize selective enrichment of pollutants in the petrochemical wastewater, and meets the specification of the COD value of the discharged wastewater in GB 31571-2015.
Description
Technical Field
The invention relates to the field of sewage treatment, in particular to an adsorption material for petrochemical sewage treatment and a preparation method thereof.
Background
The petrochemical wastewater has complex components, and organic compounds such as aromatic compounds, aromatic amines and the like contained in the wastewater have high content and high toxicity, and the COD value of the wastewater can be reduced to 100mg/L by adopting a current common water treatment method, but the wastewater has great difficulty in meeting the requirement on the COD value of the wastewater (the highest COD value is 50 mg/L) in the emission standard of pollutants in petrochemical industry (GB 31571-2015).
Adsorption is a common method of treating wastewater. For general domestic sewage, porous materials such as activated carbon have good adsorption effect, but the effect is not obvious for advanced treatment of petrochemical sewage with higher oil content and more complex components.
CN110465267a discloses a method for preparing porous adsorbent material rich in nitrogen and sulfur from oil sand asphaltene and application thereof. The method takes asphaltene extracted from oil sand as a raw material, adopts pyrolysis and chemical activation modes to prepare the carbon-based adsorbent material, and the adsorbent material obtained by the method is generally only suitable for adsorption of dye wastewater and organic salt solution, and cannot achieve good adsorption effect on petrochemical wastewater.
CN111604033a discloses an adsorbing material and a method for treating pollutants, wherein asphaltene and microorganism are combined in the method to decompose organic pollutants, and the COD of petrochemical sewage is difficult to be reduced to below 50mg/L by the adsorbing material obtained by the method.
In summary, although there are related applications of asphaltenes in the field of adsorption materials, the adsorption materials are generally obtained by pyrolysis of asphaltenes, and can only be used for treating general wastewater, so that it is difficult to effectively reduce COD of petrochemical wastewater.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an asphaltene-based adsorbing material, a preparation method and application thereof, asphaltene treated by the specific method can be used as an adsorbing material, and the asphaltene-based adsorbing material is used for treating petrochemical wastewater, can realize selective enrichment of pollutants in the petrochemical wastewater, and meets the specification of the COD value of the discharged wastewater in GB 31571-2015.
The first aspect of the present invention provides a method for preparing an asphaltene-based adsorbent material, the method comprising the steps of:
(a) Mixing asphaltenes with toluene to obtain a first mixture, and mixing a stripping agent with toluene to obtain a second mixture;
(b) Uniformly mixing the first mixture and the second mixture obtained in the step (a), and then standing and filtering to obtain a precipitate;
(c) Washing and drying the precipitate obtained in the step (b), and then mixing with chloroform to obtain a third mixture;
(d) Extracting the third mixture obtained in step (c) with an activator solution;
(e) Mixing the material obtained after the extraction in the step (d) with polyethylene glycol, extruding, forming and post-treating to obtain the asphaltene-based adsorption material.
Further, in the step (a), the asphaltenes are asphaltenes obtained by separating at least one of heavy oil, vacuum residuum, asphalt, etc.; such as a standard four-component separation procedure.
Further, in the step (a), the stripping agent is at least one of p-nitrophenol and toluene-n-heptane.
Further, in step (a), the mass ratio of asphaltenes to toluene in the first mixture is 1: 40-75. The mass ratio of the stripping agent to toluene in the second mixture is 1: 50-75.
Further, in the step (b), the first mixture and the second mixture are mixed so that the mass ratio of the asphaltenes to the stripping agent is 1-2: 1.
further, in the step (b), the standing time is generally 1 to 5 days.
In step (c), toluene is used for washing, and the washing is generally carried out for 2-5 times. The drying temperature is 20-90 ℃, and the drying time is 1-8 hours. The mass ratio of the chloroform to the precipitate is generally 40-60: 1.
further, in the step (d), the activator solution is at least one of NaOH solution and KOH solution. The mass concentration of the activator solution is 3-9 wt%.
Further, in the step (d), the amount of the activator solution is 2 to 3 times the volume of the third mixture. The extraction is generally carried out at room temperature for 3-5 hours.
Further, in the step (e), the polyethylene glycol is one or more of polyethylene glycol 200, polyethylene glycol 400 or polyethylene glycol 600; the dosage of the polyethylene glycol is 0.3% -0.5% of the total mass of the materials obtained after the extraction in the step (d).
Further, in step (e), the asphaltene-based adsorption material is obtained by washing, filtering and drying after molding. The washing is preferably carried out in water for 1-3 days.
In a second aspect the present invention provides an asphaltene-based adsorbent material prepared by the method described above.
In a third aspect, the present invention provides the use of an asphaltene-based adsorbent material prepared by the method described above in petrochemical wastewater.
Further, the petrochemical wastewater is further low-COD petrochemical wastewater, and the COD is lower than 120mg/L, preferably 70-110 mg/L.
Further, after the petrochemical sewage is subjected to adsorption treatment, the COD (chemical oxygen demand) reaches below 50 mg/L.
Compared with the prior art, the invention has the following advantages:
according to the preparation method of the asphaltene-based adsorption material, the asphaltene is subjected to a series of specific treatments, and the finally obtained asphaltene-based adsorption material has a specific adsorption effect on organic pollutants in petrochemical wastewater, so that the COD value of the petrochemical wastewater can be effectively reduced to be lower than 50mg/L, and the GB31571-2015 emission standard is met.
Detailed Description
The following detailed description of the preparation method of the adsorption material of the present invention is only for illustrating the present invention and is not limited to the technical scheme described in the embodiments of the present invention. It will be understood by those skilled in the art that the present invention may be modified or substituted for elements thereof to achieve the same technical effects, and such modifications or substituted for elements thereof should be considered as well within the scope of the present invention.
Example 1
8g of asphaltenes from a standard four component separation of heavy oil were mixed with 400g of toluene and 6g of para-nitrophenol were mixed with 400g of toluene. The two mixtures were mixed and allowed to stand for 2 days, and the lower precipitate was filtered off, washed 3 times with 400g of toluene, dried at 30℃for 5 hours and then mixed with 400g of chloroform. Extracting with 3wt% NaOH aqueous solution, wherein the amount of NaOH aqueous solution is 3 times of the volume of the mixture, extracting at room temperature for 3.5h, adding polyethylene glycol 600 accounting for 0.3% of the mass of the extract after extracting, stirring uniformly at room temperature for 5h, transferring to an extruder, extruding at room temperature under 3MPa, granulating, soaking in clear water for 3 days, filtering, and drying at 50 ℃ to obtain the asphaltene-based adsorbing material, namely PA1.
Example 2
10g of asphaltenes from a standard four component separation of vacuum residuum were mixed with 600g of toluene, 8g of toluene-n-heptane were mixed with 600g of toluene. The two mixtures were mixed and allowed to stand for 3 days, the lower precipitate was filtered off, washed 5 times with 400g of toluene, dried at 50℃for 3 hours and then mixed with 600g of chloroform. Extracting with 5wt% NaOH aqueous solution, wherein the amount of NaOH aqueous solution is 3 times of the volume of the mixture, extracting at room temperature for 5h, adding polyethylene glycol 200 accounting for 0.5% of the mass of the extract after extracting, stirring at room temperature for 3h, transferring to an extruder, extruding at room temperature under 5MPa, granulating, soaking in clear water for 1 day, filtering, and drying at 30 ℃ to obtain the asphaltene-based adsorbing material, namely PA2.
Example 3
9g of asphaltenes from standard four component separation of bitumen are mixed with 500g of toluene and 7g of para-nitrophenol are mixed with 500g of toluene. The two mixtures were mixed and allowed to stand for 2.5 days, the lower precipitate was filtered off, washed 4 times with 500g of toluene, dried for 4 hours at 40℃and then mixed with 500g of chloroform. Then extracted with 4% aqueous NaOH. The amount of NaOH aqueous solution is 2 times of the volume of the mixture, the extraction is carried out at room temperature for 4 hours, polyethylene glycol 400 accounting for 0.4% of the mass of the extract is added after the extraction, the mixture is stirred uniformly for 4 hours at room temperature and then transferred into an extruder, extruded and granulated at 4MPa at room temperature, soaked in clear water for 2 days, filtered and dried at 40 ℃ to obtain the asphaltene-based adsorption material, which is marked as PA3.
Comparative example 1
Mixing 8g of asphaltene obtained by separating heavy oil by standard four components with 400g of toluene, mixing 3g of p-nitrophenol with 400g of toluene, mixing the two obtained mixtures, standing for 2 days, and filtering to remove a lower precipitate; the obtained precipitate is washed 3 times by 400g of toluene, is mixed with 400g of chloroform after being dried for 5 hours at 30 ℃, is finally extracted by 3wt% of NaOH aqueous solution, the dosage of the NaOH aqueous solution is 3 times of the volume of the mixture, the extraction is carried out at room temperature for 3.5 hours, the extraction time is dried and transferred into an extruder, the mixture is extruded at the room temperature of 3MPa, granulated and soaked in clear water for 3 days, and is filtered and dried at 50 ℃ to obtain the asphaltene-based adsorbing material, which is marked as B1.
Comparative example 2
3g of asphaltene separated from oil sand (refer to asphaltene obtained in example 1 of CN 110465267A) was taken, and nitrogen was introduced for more than 30 minutes to ensure the inertness of the atmosphere. The temperature is controlled to rise at 5 ℃/min, and after the temperature reaches 600 ℃, the temperature is kept for 60min. And respectively collecting gas-phase products and liquid-phase products, and carrying out later separation and utilization. The pyrolyzed asphaltene coke and the activator potassium hydroxide are respectively ground in a mortar and are sieved by a 100-mesh sieve. 1g of coke powder and 2g of activator powder are respectively taken and fully mixed (stirring is carried out for more than 30 min) according to the requirement, and 0.033g of binder (Indonesia oil sand asphalt oil) is added. And (3) sampling the mixed powder for multiple times, placing the powder into a die, extruding and forming under 15MPa, blowing nitrogen for more than 30min on the formed sample, heating to 800 ℃ at a heating rate of 5 ℃/min, and keeping the temperature constant for 30min. After the sample was taken out, the sample was mixed with 200mL of 1mol/L hydrochloric acid solution and magnetically stirred for 12 hours. Standing for 1h, performing suction filtration and washing until the pH value of washing water is=7, and putting the washing water into an oven for drying to obtain a porous adsorbent material, which is marked as B2.
Test case
And evaluating the performance of the adsorbent in treating the low COD petrochemical sewage by adopting a static adsorption method. 0.5g of the adsorbents PA1, PA2, PA3, B1 and B2 and the commercially available conventional adsorbents (coconut activated carbon, fruit shell activated carbon and wood activated carbon) are weighed, respectively added into conical flasks filled with 50mL of petrochemical wastewater, placed into a constant-temperature oscillator to oscillate at constant temperature of 298.15K for 24 hours, and the supernatant is taken to measure the COD value by the method described in HJ 828-2017. The static adsorption results of the above products are shown in Table 1.
TABLE 1 results of petrochemical wastewater static adsorption
| CODmg/L before treatment | CODmg/L after treatment | COD after 5 times of cyclic use, mg/L | |
| PA1 | 103 | 26 | 29 |
| PA2 | 98 | 25 | 27 |
| PA3 | 105 | 27 | 30 |
| B1 | 103 | 53 | 75 |
| B2 | 103 | 61 | 78 |
| Coconut shell activated carbon | 103 | 57 | 80 |
| Shell active carbon | 105 | 56 | 85 |
| Wooden active carbon | 98 | 55 | 80 |
The result shows that after the asphaltene-based adsorbent for treating the low-COD petrochemical wastewater obtained through the process is treated, the COD value of the petrochemical wastewater is reduced to below 30mg/L, and the emission standard of GB31571-2015 is met.
Claims (10)
1. A method of preparing an asphaltene-based adsorbent material, the method comprising the steps of:
(a) Mixing asphaltenes with toluene to obtain a first mixture, and mixing a stripping agent with toluene to obtain a second mixture;
(b) Uniformly mixing the first mixture and the second mixture obtained in the step (a), and then standing and filtering to obtain a precipitate;
(c) Washing and drying the precipitate obtained in the step (b), and then mixing with chloroform to obtain a third mixture;
(d) Extracting the third mixture obtained in step (c) with an activator solution;
(e) Mixing the material obtained after the extraction in the step (d) with polyethylene glycol, extruding, forming and post-treating to obtain an asphaltene-based adsorption material;
in the step (a), the stripping agent is at least one of p-nitrophenol and toluene-n-heptane;
in the step (d), the activator solution is at least one of NaOH solution and KOH solution.
2. A method according to claim 1, characterized in that: in step (a), the mass ratio of asphaltenes to toluene in the first mixture is 1: 40-75, wherein the mass ratio of the stripping agent to toluene in the second mixture is 1: 50-75 parts; and/or in the step (b), the mass ratio of the asphaltene to the stripping agent in the mixture of the first mixture and the second mixture is 1-2: 1.
3. a method according to claim 1, characterized in that: in the step (a), the asphaltenes are at least one asphaltenes obtained by separating heavy oil, vacuum residuum and asphalt.
4. A method according to claim 1, characterized in that: in step (c), the washing is performed with toluene; the mass ratio of the chloroform to the precipitate is 40-60: 1.
5. a method according to claim 1, characterized in that: the mass concentration of the activator solution is 3-9 wt%.
6. A method according to claim 1, characterized in that: in the step (d), the use amount of the activator solution is 2-3 times of the volume of the third mixture, and the extraction time is 3-5 hours.
7. A method according to claim 1, characterized in that: in the step (e), the polyethylene glycol is one or more of polyethylene glycol 200, polyethylene glycol 400 or polyethylene glycol 600; the dosage of the polyethylene glycol is 0.3% -0.5% of the total mass of the materials obtained after the extraction in the step (d).
8. A method according to claim 1, characterized in that: in the step (e), the asphaltene-based adsorption material is obtained after the molding, washing, filtering and drying.
9. An asphaltene-based adsorbent material, characterized in that: prepared by the method of any one of claims 1-8.
10. Use of an asphaltene-based adsorbent material prepared according to the method of any one of claims 1 to 8 in petrochemical wastewater.
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| JPH09255320A (en) * | 1996-03-19 | 1997-09-30 | Maruzen Petrochem Co Ltd | Production of porous carbon material having fine pore |
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| CN107365595A (en) * | 2016-05-11 | 2017-11-21 | 中国石油化工股份有限公司 | A kind of preparation method and applications of crude oil asphaltenes |
| CN110127694A (en) * | 2019-05-17 | 2019-08-16 | 中国铝业股份有限公司 | A kind of preparation method of asphalt based active carbon |
| CN110465267A (en) * | 2019-07-08 | 2019-11-19 | 天津大学 | Oil sand asphalt texture preparation is rich in the methods and applications of nitrogen sulphur porous adsorbent material |
| CN111575048A (en) * | 2020-05-27 | 2020-08-25 | 中国科学院广州地球化学研究所 | Method for separating crude oil asphaltene subcomponents |
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| JPH09255320A (en) * | 1996-03-19 | 1997-09-30 | Maruzen Petrochem Co Ltd | Production of porous carbon material having fine pore |
| CN107365595A (en) * | 2016-05-11 | 2017-11-21 | 中国石油化工股份有限公司 | A kind of preparation method and applications of crude oil asphaltenes |
| CN106590719A (en) * | 2016-11-15 | 2017-04-26 | 天津海威欧能源科技有限责任公司 | Oil sand asphalt solvent extraction separation system and process |
| CN110127694A (en) * | 2019-05-17 | 2019-08-16 | 中国铝业股份有限公司 | A kind of preparation method of asphalt based active carbon |
| CN110465267A (en) * | 2019-07-08 | 2019-11-19 | 天津大学 | Oil sand asphalt texture preparation is rich in the methods and applications of nitrogen sulphur porous adsorbent material |
| CN111575048A (en) * | 2020-05-27 | 2020-08-25 | 中国科学院广州地球化学研究所 | Method for separating crude oil asphaltene subcomponents |
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Effective date of registration: 20231229 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |