CN115532233A - Asphaltene-based adsorption material and preparation method and application thereof - Google Patents
Asphaltene-based adsorption material and preparation method and application thereof Download PDFInfo
- Publication number
- CN115532233A CN115532233A CN202110723572.2A CN202110723572A CN115532233A CN 115532233 A CN115532233 A CN 115532233A CN 202110723572 A CN202110723572 A CN 202110723572A CN 115532233 A CN115532233 A CN 115532233A
- Authority
- CN
- China
- Prior art keywords
- mixture
- asphaltene
- toluene
- mixing
- polyethylene glycol
- 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.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 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 45
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 19
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000605 extraction Methods 0.000 claims abstract description 16
- 239000002244 precipitate Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000012190 activator Substances 0.000 claims abstract description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000003463 adsorbent Substances 0.000 claims description 11
- 239000002351 wastewater Substances 0.000 claims description 11
- 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 5
- 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
- 230000003213 activating effect Effects 0.000 claims description 2
- 239000010865 sewage Substances 0.000 abstract description 20
- 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 16
- 239000000243 solution Substances 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
- 238000000926 separation method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003027 oil sand Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000003068 static effect Effects 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
- PFRUBEOIWWEFOL-UHFFFAOYSA-N [N].[S] Chemical compound [N].[S] PFRUBEOIWWEFOL-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 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
- 238000001125 extrusion Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000197 pyrolysis Methods 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
- 238000007873 sieving Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- -1 vacuum residue Substances 0.000 description 1
Classifications
-
- 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)
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Civil Engineering (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Liquids With Adsorbents In General (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 and toluene to obtain a first mixture, and mixing a stripping agent and the toluene to obtain a second mixture; (b) Uniformly mixing the first mixture and the second mixture obtained in the step (a), standing and filtering to obtain a precipitate; (c) Washing and drying the precipitate obtained in the step (b), and mixing the precipitate with chloroform to obtain a third mixture; (d) Extracting the third mixture from step (c) with an activator solution; (e) And (d) mixing the material obtained after the extraction in the step (d) with polyethylene glycol, extruding, molding, and performing post-treatment to obtain the asphaltene-based adsorbing material. The asphaltene-based adsorption material is used for treating petrochemical sewage, can realize selective enrichment of pollutants in the petrochemical sewage, and meets the regulation of COD value of external sewage in GB 31571-2015.
Description
Technical Field
The invention relates to the field of sewage treatment, in particular to an adsorbing material for petrochemical sewage treatment and a preparation method thereof.
Background
Petrochemical wastewater is complex in components, and organic compounds such as aromatic hydrocarbon compounds and aromatic amines contained in the petrochemical wastewater are high in content and toxicity, so that the COD value of the wastewater can be reduced to 100mg/L by adopting a current common water treatment method, but the treatment method has great difficulty in meeting the requirements (the highest COD value is 50 mg/L) in discharge Standard of pollutants for petrochemical industry (GB 31571-2015).
Adsorption processes are common methods for treating wastewater. For general domestic sewage, porous materials such as activated carbon and the like have good adsorption effect, but for advanced treatment of petrochemical sewage with higher oil content and more complex components, the effect is not obvious.
CN110465267A discloses a method for preparing a nitrogen-sulfur-rich porous adsorbent material from oil sand asphaltene and application of the nitrogen-sulfur-rich porous adsorbent material. The method takes asphaltene extracted from oil sand as a raw material, prepares a carbon-based porous adsorbent material by adopting a pyrolysis and chemical activation mode, and the adsorbing material obtained by the method is generally only suitable for adsorption of dye wastewater and organic salt solution, and cannot achieve a good adsorption effect on petrochemical wastewater.
CN111604033A discloses an adsorbing material and a method for treating pollutants, the method needs to combine asphaltene and microorganisms to decompose organic pollutants, and the adsorbing material obtained by the method is difficult to reduce the COD of petrochemical sewage to below 50 mg/L.
In summary, although there are applications related to the use of asphaltenes in the field of adsorption materials, the adsorption materials are generally obtained by pyrolyzing asphaltenes, and can only be used for treating general wastewater, and it is difficult to effectively reduce the COD of petrochemical wastewater.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an asphaltene-based adsorption material and a preparation method and application thereof, wherein the asphaltene treated by the specific method can be used as the adsorption material, and the asphaltene-based adsorption material is used for treating petrochemical sewage, can realize the selective enrichment of pollutants in the petrochemical sewage, and meets the regulation of COD value of external sewage in GB 31571-2015.
In a first aspect, the present invention provides a method for preparing an asphaltene-based adsorption material, comprising the steps of:
(a) Mixing asphaltenes and toluene to obtain a first mixture, and mixing a stripping agent and the toluene to obtain a second mixture;
(b) Uniformly mixing the first mixture and the second mixture obtained in the step (a), standing and filtering to obtain a precipitate;
(c) Washing and drying the precipitate obtained in the step (b), and mixing the precipitate with chloroform to obtain a third mixture;
(d) Extracting the third mixture from step (c) with an activator solution;
(e) And (d) mixing the material obtained after the extraction in the step (d) with polyethylene glycol, extruding, molding, and performing post-treatment to obtain the asphaltene-based adsorbing material.
Further, in the step (a), the asphaltene is at least one separated asphaltene in heavy oil, vacuum residue, asphalt and the like; such as using 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 the asphaltenes to the toluene in the first mixture is 1:40 to 75. The mass ratio of the stripping agent to the toluene in the second mixture is 1:50 to 75.
Further, in 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 step (b), the standing time is typically 1~5 days.
Further, in step (c), the washing is performed with toluene, typically 2~5 times. The drying temperature is 20 to 90 ℃, and the drying time is 1 to 8h. The mass ratio of the chloroform dosage to the precipitate is generally 40 to 60:1.
further, in the step (d), the activator solution is at least one of a NaOH solution and a KOH solution. The mass concentration of the activator solution is 3-9 wt%.
Further, in step (d), the amount of activator solution used is 2~3 times the volume of the third mixture. The extraction is generally carried out at room temperature for an extraction time of 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 the step (e), the formed product is washed, filtered and dried to obtain the asphaltene-based adsorbing material. The wash is preferably soaked in water for 1~3 days.
In a second aspect, the present invention provides an asphaltene-based adsorbent material prepared by the above method.
In a third aspect, the invention provides the use of an asphaltene-based adsorption material prepared by the above method in petrochemical wastewater.
Further, the petrochemical sewage is low COD petrochemical sewage, and the COD is less than 120mg/L, preferably 70 to 110mg/L.
Further, after the petrochemical sewage is subjected to adsorption treatment, the COD 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 treatment, and the finally obtained asphaltene-based adsorption material has a specific adsorption effect on organic pollutants in petrochemical sewage, so that the COD value of the petrochemical sewage can be effectively reduced to be below 50mg/L, and the discharge standard of GB31571-2015 is met.
Detailed Description
The following detailed description of the method for preparing the adsorbent material of the present invention is only for illustrating the present invention and is not limited to the technical solutions described in the embodiments of the present invention. It will be appreciated by those skilled in the art that modifications and equivalents may be made to the invention as long as they achieve the same technical result, and such modifications and equivalents should be considered as falling within the scope of the invention.
Example 1
8g of asphaltenes obtained by standard four component separation of heavy oil were mixed with 400g of toluene, 6g of p-nitrophenol was mixed with 400g of toluene. The two mixtures were mixed and allowed to stand for 2 days, the lower precipitate was filtered off and washed 3 times with 400g of toluene, then dried at 30 ℃ for 5 hours and mixed with 400g of chloroform. And then extracting with 3wt% of NaOH aqueous solution, wherein the amount of the NaOH aqueous solution is 3 times of the volume of the mixture, the extraction is carried out at room temperature, the extraction time is 3.5h, polyethylene glycol 600 accounting for 0.3% of the mass of the extract is added after the extraction, the mixture is uniformly stirred for 5h at room temperature and then transferred into an extruder, the mixture is extruded and granulated at room temperature under 3MPa, and is soaked in clear water for 3 days, and then the mixture is filtered and dried at 50 ℃ to obtain the asphaltene-based adsorbing material, namely PA1.
Example 2
10g of asphaltenes obtained by standard four-component separation of vacuum residue were mixed with 600g of toluene, 8g of toluene-n-heptane and 600g of toluene. The two mixtures were mixed and allowed to stand for 3 days, the lower precipitate was filtered off and washed 5 times with 400g of toluene, then dried at 50 ℃ for 3 hours and mixed with 600g of chloroform. And extracting with 5wt% of NaOH aqueous solution, wherein the amount of the NaOH aqueous solution is 3 times of the volume of the mixture, the extraction is carried out at room temperature, the extraction time is 5h, polyethylene glycol 200 accounting for 0.5% of the mass of the extract is added after the extraction, the mixture is stirred for 3h at room temperature and then transferred into an extruder, the mixture is extruded and granulated at room temperature under 5MPa, and is soaked in clear water for 1 day, and then the mixture is filtered and dried at 30 ℃ to obtain the asphaltene-based adsorbing material, namely PA2.
Example 3
9g of asphaltenes obtained by subjecting the bitumen to standard four-component separation were mixed with 500g of toluene and 7g of p-nitrophenol was mixed with 500g of toluene. The two mixtures were mixed and allowed to stand for 2.5 days, the lower precipitate was filtered off and washed 4 times with 500g of toluene, then dried at 40 ℃ for 4 hours and mixed with 500g of chloroform. And extracted with 4% aqueous NaOH. And the using amount of the 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 percent of the mass of the extract is added after the extraction, the mixture is uniformly stirred at room temperature for 4 hours and then transferred into an extruder, the mixture is extruded and granulated at room temperature under 4MPa and is soaked in clear water for 2 days, and then the mixture is filtered and dried at 40 ℃ to obtain the asphaltene-based adsorbing material, namely PA3.
Comparative example 1
Mixing 8g of asphaltene obtained by separating heavy oil from standard four components with 400g of toluene, mixing 3g of p-nitrophenol with 400g of toluene, mixing the two mixtures, standing for 2 days, and filtering to obtain lower-layer precipitate; washing the obtained precipitate with 400g of toluene for 3 times, drying at 30 ℃ for 5 hours, mixing with 400g of chloroform, extracting with 3wt% of NaOH aqueous solution, wherein the amount of the NaOH aqueous solution is 3 times of the volume of the mixture, extracting at room temperature for 3.5 hours, drying, transferring into 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, which is marked as B1.
Comparative example 2
3g of asphaltenes separated from the oil sand (asphaltenes obtained in example 1 referred to in CN 110465267A) were taken and nitrogen was passed over 30min to ensure inertness of the atmosphere. Controlling the temperature to rise at 5 ℃/min, and keeping the temperature for 60min after the temperature reaches 600 ℃. And respectively collecting the gas-phase product and the liquid-phase product, and performing later separation and utilization. And (3) grinding the pyrolyzed asphaltene coke and the activating agent potassium hydroxide in a mortar respectively, and sieving by using a 100-mesh sieve. 1g of coke powder and 2g of activator powder are respectively taken according to the requirement, fully mixed (stirred for more than 30 min), and 0.033g of binder (Indonesia oil sand asphalt oil) is added. And sampling the mixed powder for multiple times, putting the mixed powder into a die, carrying out extrusion forming under 15MPa, carrying out nitrogen purging on the formed sample for more than 30min, heating to 800 ℃ at a heating rate of 5 ℃/min, and keeping the constant temperature for 30min. After the sample was taken out, the sample was mixed with 200mL of a 1mol/L hydrochloric acid solution and magnetically stirred for 12 hours. Standing for 1h, performing suction filtration and washing until the pH of the washing water is =7, and putting the washing water into an oven for drying to obtain the porous adsorbent material, which is recorded as B2.
Test example
The performance of the adsorbent for treating low-COD petrochemical sewage is evaluated by adopting a static adsorption method. 0.5g of the adsorbents PA1, PA2, PA3 and B1 and B2 of the invention and conventional adsorbents (coconut shell activated carbon, fruit shell activated carbon and wood activated carbon) sold in the market are respectively added into a conical flask filled with 50mL of petrochemical sewage, the conical flask is placed into a constant temperature oscillator to be subjected to constant temperature oscillation at 298.15K for 24 hours, and then the supernatant is taken to measure the COD value by adopting the method of HJ 828-2017. The results of the static adsorption of the above product are shown in Table 1.
TABLE 1 static adsorption results for petrochemical wastewater
| CODmg/L before treatment | Treated CODmg/L | COD, mg/L after 5 times of cyclic use | |
| 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 |
| Husk activated carbon | 105 | 56 | 85 |
| Wood activated carbon | 98 | 55 | 80 |
The results show that after the asphalt-based adsorbent for treating the low-COD petrochemical sewage obtained by the process is treated, the COD value of the petrochemical sewage is reduced to be below 30mg/L, and the discharge standard of GB31571-2015 is met.
Claims (11)
1. A method for preparing an asphaltene-based adsorption material, comprising the steps of:
(a) Mixing asphaltene and toluene to obtain a first mixture, and mixing a stripping agent and the toluene to obtain a second mixture;
(b) Uniformly mixing the first mixture and the second mixture obtained in the step (a), standing and filtering to obtain a precipitate;
(c) Washing and drying the precipitate obtained in the step (b), and mixing the precipitate with chloroform to obtain a third mixture;
(d) Extracting the third mixture from step (c) with an activator solution;
(e) And (d) mixing the material obtained after the extraction in the step (d) with polyethylene glycol, extruding, molding, and performing post-treatment to obtain the asphaltene-based adsorbing material.
2. The method of claim 1, wherein: 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 the toluene in the second mixture is 1:50 to 75; and/or, in step (b), the mass ratio of the asphaltenes to the stripping agent in the first mixture and the second mixture is 1~2:1.
3. the method of claim 1, wherein: in the step (a), the asphaltene is at least one separated asphaltene in heavy oil, vacuum residue and asphalt.
4. The method of claim 1, wherein: in the step (a), the stripping agent is at least one of p-nitrophenol and toluene-n-heptane.
5. The method of claim 1, wherein: in the step (c), the washing is carried out by adopting toluene; the mass ratio of the chloroform dosage to the precipitate is 40-60: 1.
6. the method of claim 1, wherein: in the step (d), the activating agent solution is at least one of NaOH solution and KOH solution; the mass concentration of the activator solution is 3wt% -9 wt%.
7. The method of claim 1, wherein: in step (d), the amount of activator solution used was 2~3 times the volume of the third mixture, and the extraction time was 3~5 hours.
8. The method of claim 1, wherein: 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).
9. The method of claim 1, wherein: and (e) washing, filtering and drying after forming to obtain the asphaltene-based adsorbing material.
10. An asphaltene-based adsorbent material, characterized in that: prepared by the process of any one of claims 1 to 9.
11. Use of an asphaltene-based adsorption material prepared according to the method according to any one of claims 1-9 in petrochemical wastewater.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110723572.2A CN115532233B (en) | 2021-06-29 | 2021-06-29 | Asphaltene-based adsorption material, and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110723572.2A CN115532233B (en) | 2021-06-29 | 2021-06-29 | Asphaltene-based adsorption material, and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115532233A true CN115532233A (en) | 2022-12-30 |
| CN115532233B CN115532233B (en) | 2023-07-28 |
Family
ID=84716721
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110723572.2A Active CN115532233B (en) | 2021-06-29 | 2021-06-29 | Asphaltene-based adsorption material, and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115532233B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09255320A (en) * | 1996-03-19 | 1997-09-30 | Maruzen Petrochem Co Ltd | Production of porous carbon material having fine pore |
| 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 |
| 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 |
-
2021
- 2021-06-29 CN CN202110723572.2A patent/CN115532233B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115532233B (en) | 2023-07-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP1200343B1 (en) | Method for producing shaped, activated charcoal | |
| CN109433153B (en) | Nano lanthanum hydroxide modified lignin porous carbon and preparation method and application thereof | |
| CN113559824B (en) | Nitrogen-doped porous carbon material adsorbent for treating dye wastewater and preparation method and application thereof | |
| CN105597691A (en) | Preparation method and application of composite microspheres | |
| CN108467036B (en) | Desiliconized rice hull-based activated carbon and preparation method and application thereof | |
| CN113976050B (en) | Preparation method of magnetic cellulose-graphene oxide high-adsorptivity aerogel | |
| CN110898802B (en) | Sludge-based biochar and preparation method and application thereof, acetic acid modified sludge-based biochar and preparation method and application thereof | |
| CN106589168A (en) | Beta-cyclodextrin compound, preparation method thereof, and application thereof in water treatment | |
| CN111530386A (en) | Preparation method of antibacterial amidoxime aerogel for extracting uranium from seawater | |
| CN108435135A (en) | A kind of preparation method of watermelon peel charcoal and its in removing waste water thallium application | |
| CN113634229A (en) | Preparation method and application of biochar with selective adsorption-desorption capacity | |
| CN113289578B (en) | Gasified slag-based composite ammonia nitrogen adsorbent, preparation method and regeneration method thereof, application thereof and method for treating ammonia nitrogen-containing wastewater | |
| KR20160085034A (en) | Method for preparing adsorbent for removing stench gas from waste and the adsorbent for removing stench gas thereby | |
| CN113477226A (en) | Method for removing trivalent antimony in aqueous solution by using chitosan modified charcoal | |
| CN115532233B (en) | Asphaltene-based adsorption material, and preparation method and application thereof | |
| CN111533127B (en) | Efficient modified activated carbon capable of adsorbing various VOC gases and preparation method thereof | |
| CN110508268B (en) | Activation regeneration method of decolorized sand | |
| CN105170107B (en) | A kind of preparation method of green heavy metal chelating agent | |
| CN110368897B (en) | Coal tar-based nitrogen-containing porous carbon with ultrahigh specific surface area as well as preparation method and application thereof | |
| CN111298761B (en) | Modified sepiolite adsorbent and preparation method and application thereof | |
| CN116474748A (en) | Modified biochar and application thereof in cadmium and arsenic polluted soil | |
| CN113213579B (en) | Application of photocatalytic biochar composite material in catalytic degradation of printing and dyeing wastewater | |
| CN115532232B (en) | Asphaltene-based adsorbent and preparation method and application thereof | |
| CN110203930B (en) | Activated carbon and preparation method thereof | |
| CN111841485B (en) | Preparation method of carbonized modified red mud ceramsite adsorbent, and regeneration method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
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. |