CN116510690A - Hydrophobic biochar composite material and preparation method thereof - Google Patents
Hydrophobic biochar composite material and preparation method thereof Download PDFInfo
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- CN116510690A CN116510690A CN202310558494.4A CN202310558494A CN116510690A CN 116510690 A CN116510690 A CN 116510690A CN 202310558494 A CN202310558494 A CN 202310558494A CN 116510690 A CN116510690 A CN 116510690A
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- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 102
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000003344 environmental pollutant Substances 0.000 claims abstract description 35
- 231100000719 pollutant Toxicity 0.000 claims abstract description 35
- 238000001179 sorption measurement Methods 0.000 claims abstract description 30
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229920001577 copolymer Polymers 0.000 claims abstract description 22
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- BCAIDFOKQCVACE-UHFFFAOYSA-N 3-[dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azaniumyl]propane-1-sulfonate Chemical compound CC(=C)C(=O)OCC[N+](C)(C)CCCS([O-])(=O)=O BCAIDFOKQCVACE-UHFFFAOYSA-N 0.000 claims abstract description 16
- PSBDWGZCVUAZQS-UHFFFAOYSA-N (dimethylsulfonio)acetate Chemical compound C[S+](C)CC([O-])=O PSBDWGZCVUAZQS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229940117986 sulfobetaine Drugs 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 12
- 230000010355 oscillation Effects 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 239000000356 contaminant Substances 0.000 claims 9
- 239000000463 material Substances 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 239000003999 initiator Substances 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 239000002023 wood Substances 0.000 description 5
- -1 Perfluoro compounds Chemical class 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 3
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 208000008839 Kidney Neoplasms Diseases 0.000 description 1
- 229920006926 PFC Polymers 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 208000014018 liver neoplasm Diseases 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid 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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
-
- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the technical field of environment new functional materials, and discloses a hydrophobic biochar composite material and a preparation method thereof, wherein the hydrophobic biochar composite material comprises biochar, and the surface of the biochar is modified with a copolymer of sulfobetaine and acrylamide; the preparation method of the hydrophobic biochar composite material comprises the following steps: the preparation method comprises the steps of taking acrylamide and [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide as raw materials, taking ammonium persulfate as an initiator, taking N, N, N, N-tetramethyl ethylenediamine as an accelerator, preparing a copolymer of sulfobetaine and acrylamide, modifying the copolymer on the surface of biochar through physical adsorption and chemical action, specifically putting the biochar into a mixed solution of acrylamide and [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide, introducing nitrogen to deoxidize, then adding ammonium persulfate and N, N, N, N-tetramethyl ethylenediamine to react, generating the copolymer of sulfobetaine and acrylamide, and loading the copolymer on the surface of the biochar to obtain the hydrophobic biochar composite material. The hydrophobic biochar composite material provided by the invention has the advantages of hydrophobicity, strong adsorption capacity, high practical application value and the like, can be used for adsorbing hydrophobic pollutants in water, and is a novel biochar material with great prospect.
Description
Technical Field
The invention belongs to the technical field of new environment functional materials, and particularly relates to a hydrophobic biochar composite material and a preparation method thereof.
Background
Perfluoro compounds (pfases) have found widespread use in industry over the past decades, but are ubiquitous in the environment due to their chemical durability. Exposure to pfases presents serious health risks, such as liver and kidney cancers, and thus such compounds are now considered primary pollutants. Among the methods currently used for the removal of PFCs, adsorption is considered one of the most suitable techniques.
The biochar has adjustable specific surface area and pore structure, the surface of the biochar has rich functional groups, the biochar can be obtained by pyrolysis of various biomass materials at high temperature, and the prepared raw materials are wide in source and are low-cost, widely available and environment-friendly materials. The surface of the biochar is rich in oxygen-containing functional groups such as-COOH, -CHO, -OH and the like, so that the biochar has good adsorption effect on a plurality of substances. However, these oxygen-containing functional groups are relatively hydrophilic and are limited in their adsorption of hydrophobic materials. Therefore, how to improve the hydrophobicity of the biochar has great significance for effectively removing the pollutant with hydrophobicity.
Through the above analysis, the problems and defects existing in the prior art are as follows: when the oxygen-containing functional groups such as-COOH, -CHO, -OH and the like which are rich on the surface of the biochar are hydrophilic groups and adsorb hydrophobic pollutants, the hydrophilic and hydrophobic properties of the two can prevent the adsorption from being carried out, and the removal effect of the biochar on the hydrophobic pollutants is affected. The prior modification technology improves the adsorption performance of the biochar by mainly changing the ash content and the type of functional groups of the biochar and improving the pore structure of the biochar. However, these modification techniques cannot change the hydrophobicity of biochar. Therefore, the prior modification technology cannot greatly improve the removal effect of the biochar on the hydrophobic pollutants. The scheme for preparing the hydrophobic biochar material in the prior art has not been reported in the prior art.
The difficulty of solving the problems and the defects is as follows: the hydrophobic effect between the biochar and the pollutant is involved in the adsorption of the hydrophobic pollutant, and the stronger the biochar is, the stronger the hydrophobic effect between the biochar and the pollutant is, and the better the adsorption effect is. Although modification technology aiming at physical and chemical properties of the biochar is endlessly layered at present, the modification technology mainly comprises the steps of changing the pore structure of the biochar and introducing hydrophilic groups. The prior modification technology can not improve the hydrophobicity of the biochar.
The meaning of solving the problems and the defects is as follows: is beneficial to improving the adsorption effect of the biochar on the hydrophobic pollutants.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a hydrophobic biochar composite material and a preparation method thereof.
The invention is realized in such a way that a hydrophobic biochar composite material comprises biochar, the surface of which is modified with a copolymer of sulfobetaine and acrylamide.
The preparation method of the cationic polyacrylamide modified biochar composite material comprises the following steps:
step one, preparing a mixed solution of acrylamide and [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide;
step two, putting the biochar into the mixed solution obtained in the step one to obtain black suspension;
step three, introducing nitrogen into the black suspension obtained in the step two for half an hour;
step four, adding ammonium persulfate and N, N, N, N-tetramethyl ethylenediamine into the black suspension obtained in the step three to react, so as to obtain a hydrophobic biochar composite material;
in the first step, the mass volume ratio of the acrylamide to the water in the mixed solution of the acrylamide and the [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide is 10 g-20 g:100mL of [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide and water, wherein the mass volume ratio of the [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide to water is 10-40 g:100mL;
in the second step, the mass volume ratio of the biochar to the mixed solution is 10-20 g:100mL; after mixing, stirring for 6-24 h at the temperature of 20-40 ℃ and the rotating speed of 160-180 rpm.
In the third step, 100-200 mL/min nitrogen is introduced into the mixed solution, and the mixed solution is stirred for 0.5-2 h at the temperature of 50-60 ℃ and the rotating speed of 120-180 rpm;
in the fourth step, the mass volume ratio of the ammonium persulfate to the black suspension is 2 mg-20 mg:100mL, wherein the mass volume ratio of the N, N, N, N-tetramethyl ethylenediamine to the black suspension is 5 g-20 g:100mL, wherein the reaction is carried out at 50-65 ℃ under stirring at a rotating speed of 100-180 rpm for 12h.
The invention also aims to provide an application of the hydrophobic biochar composite material in adsorbing hydrophobic pollutants in a water body.
Further, the application method of the hydrophobic biochar composite material in adsorbing hydrophobic pollutants in a water body comprises the following steps:
mixing the hydrophobic biochar composite material with a water body containing hydrophobic pollutants, and carrying out oscillation treatment to complete the adsorption treatment of the hydrophobic pollutants in the water body.
The application of the hydrophobic biochar composite material in adsorbing hydrophobic pollutants in water is characterized in that the mass volume ratio of the hydrophobic biochar composite material to the water containing the hydrophobic pollutants is 0.1 g-1.0 g:1L.
The application of the hydrophobic biochar composite material in adsorbing hydrophobic pollutants in water is characterized in that the pollutants are perfluorinated compounds, and the initial concentration of the pollutants in the water containing the pollutants is 1 mg/L-100 mg/L.
The application of the hydrophobic biochar composite material in adsorbing hydrophobic pollutants in water is characterized in that the temperature of the oscillation treatment is 20-35 ℃, the rotation speed of the oscillation treatment is 150-200 rpm, and the time of the oscillation treatment is 0.5-24 h.
By combining all the technical schemes, the invention has the advantages and positive effects that: the hydrophobic biochar composite material provided by the invention comprises biochar, wherein the surface of the biochar is modified with a copolymer of sulfobetaine and acrylamide. In the invention, the copolymer of the sulfobetaine and the acrylamide not only contains a large amount of protonated groups, but also can respond to the change of temperature, the chain conformation of the copolymer is changed drastically, and the copolymer shows hydrophobicity at normal temperature. The copolymer prepared by reacting acrylamide with [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide is used for modifying biochar, is favorable for changing the hydrophobicity of an adsorption material, improves the adsorption capacity on hydrophobic pollutants, and expands the application of the biochar material in the aspect of treating polluted water. The hydrophobic biochar composite material has the advantages of being hydrophobic, strong in adsorption capacity, high in practical application value and the like, can be used for adsorbing hydrophobic pollutants in water, and is a novel biochar material with great prospect.
In the hydrophobic biological carbon composite material, as the copolymer of the sulfobetaine and the acrylamide is modified, the hydrophilicity and the hydrophobicity of the biological carbon are changed, the higher the content of the copolymer of the sulfobetaine and the acrylamide on the surface of the biological carbon is, the higher the hydrophobicity of the surface of the biological carbon is, and the higher the hydrophobic effect between the surface of the biological carbon and hydrophobic pollutants is, so that the adsorption and removal effects on the hydrophobic pollutants are better.
The invention also provides a preparation method of the hydrophobic biochar composite material, which takes acrylamide and [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide as raw materials, ammonium persulfate as an initiator, N, N, N-tetramethyl ethylenediamine as an accelerator, prepares a copolymer of sulfobetaine and acrylamide, and modifies the copolymer on the surface of the biochar through physical adsorption and chemical action, specifically puts the biochar into a mixed solution of acrylamide and [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide, and then deoxidizes by introducing nitrogen, and then adds ammonium persulfate and N, N, N-tetramethyl ethylenediamine to react to generate the copolymer of the sulfobetaine and the acrylamide, and loads the copolymer on the surface of the biochar. Therefore, the preparation method has the advantages of simple process, easy operation, mild and controllable reaction conditions, low cost, short time consumption and the like, is suitable for continuous large-scale batch production, and is convenient for industrial utilization.
The invention also provides application of the hydrophobic biochar composite material in adsorbing hydrophobic pollutants in water, and the hydrophobic biochar composite material and the hydrophobic pollutants are mixed for oscillation treatment, so that the adsorption treatment of the hydrophobic pollutants in the water can be realized. Taking a water body containing a perfluorinated compound as an example, the hydrophobic biochar composite material has stronger adsorption capacity on the perfluorinated compound in the water body, and when the initial concentration of the perfluorinated compound in the water body is 10mg/L, the adsorption capacity is improved by more than 140% compared with that of the original biochar. The hydrophobic biochar composite material has remarkable adsorption and removal effects on hydrophobic pollutants in water, is suitable for repairing polluted water, can realize effective removal of the hydrophobic pollutants, has higher application value in treating the polluted water, and has wide application prospect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flowchart of a preparation method of a hydrophobic biochar composite material provided by an embodiment of the invention.
FIG. 2 is an SEM image of a hydrophobic biochar composite prepared according to example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Aiming at the problems existing in the prior art, the invention provides a hydrophobic biochar composite material and a preparation method thereof, and the invention is described in detail below with reference to the accompanying drawings.
The hydrophobic biochar composite material provided by the embodiment of the invention comprises biochar, wherein the surface of the biochar is modified with a copolymer of sulfobetaine and acrylamide.
As shown in fig. 1, the preparation method of the hydrophobic biochar composite material provided by the embodiment of the invention comprises the following steps:
s101, preparing a mixed solution of acrylamide and [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide;
s102, putting the biochar into the mixed solution obtained in the step S101, and reacting to obtain black suspension;
and S103, reacting the black suspension obtained in the step S102 with ammonium persulfate and N, N, N, N-tetramethyl ethylenediamine to obtain the hydrophobic biochar composite material.
Other steps may be performed by those skilled in the art to prepare the hydrophobic biochar composite provided by the present invention, and the preparation method of the hydrophobic biochar composite provided by the present invention in fig. 1 is merely a specific example.
The original biochar used in the following examples was self-made and the remaining materials and instruments were commercially available. In the examples of the present invention, unless otherwise specified, the process used was a conventional process, the equipment used was a conventional equipment, and the data obtained were all averages of three or more tests.
The technical scheme of the present invention is further described below with reference to examples.
Example 1
The hydrophobic biochar composite material provided by the embodiment of the invention comprises wood chip biochar, wherein the surface of the wood chip biochar is modified with a copolymer of sulfobetaine and acrylamide.
The preparation method of the hydrophobic carbon composite material in the embodiment provided by the embodiment of the invention comprises the following steps:
(1) Cleaning wood chips with deionized water, drying at 70 ℃ for 24 hours, crushing and sieving (0.15-0.25 mm) the dried wood chips, then placing the crushed and sieved wood chips into a tube furnace for pyrolysis firing, keeping a quartz tube of the tube furnace sealed in the pyrolysis process, simultaneously introducing N2 into the tube at a flow rate of 200mL/min, so as to keep anaerobic conditions in the whole pyrolysis process, and setting a heating program of the tube furnace to be: heating from room temperature to 600 ℃ at a heating rate of 3 ℃/min, continuously pyrolyzing for 2 hours under the temperature condition, then starting a natural cooling process, continuously introducing N2 at the same flow rate in the cooling process, cooling to room temperature, taking out to obtain original biochar, and sieving the biochar to obtain biochar powder (0.15-0.25 mm).
(2) 100mL of a mixed solution of acrylamide and [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide was prepared, and the mass ratio of acrylamide to [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide was 10g:15g;
(3) 5g of biochar is put into the mixed solution in the step (2), stirred for 12 hours at the speed of 150rpm at 35 ℃, N2 is introduced into the solution at the flow rate of 100mL/min, and stirred for 1 hour at 180rpm at 35 ℃ to obtain black suspension;
(4) And (3) adding 5mg of ammonium persulfate into the black suspension in the step (3), stirring at a rotating speed of 120rpm for 12 hours at 60 ℃, filtering and collecting solids, and drying the solids to obtain the hydrophobic biochar composite material.
The hydrophobic biochar composite material prepared in the embodiment 1 of the invention has black powder appearance. The hydrophobic biochar composite prepared in example 1 of the present invention was observed under a scanning electron microscope, and the result is shown in fig. 2. Fig. 2 is an SEM image of the hydrophobic biochar composite of the present invention.
Example 2
The application of the hydrophobic biochar composite material in adsorbing hydrophobic pollutants in water, in particular to the application of the hydrophobic biochar composite material in adsorbing perfluorinated compounds in water, comprises the following steps:
the mass volume ratio of the hydrophobic biochar composite material to the water body (the water solution containing the perfluorinated compounds) is 0.1g:1L of the hydrophobic biochar composite material prepared in the example 1 is weighed, and added into a solution (the volume of the solution is 100 mL) containing perfluorooctyl sulfonic acid (hereinafter referred to as PFOS) and perfluorooctanoic acid (hereinafter referred to as PFOA) with the concentration of 10mg/L respectively, and the mixture is uniformly mixed, and subjected to constant-temperature oscillation treatment for 24 hours at the rotating speed of 180rpm and the temperature of 25 ℃ to finish the treatment of the aqueous solution containing the perfluorinated compound. After the completion of the shaking treatment, the mixture was allowed to stand for precipitation, and the concentration of the perfluoro compound was measured by HPLC-HRMS/MS to calculate the amount of perfluoro compound adsorbed by the hydrophobic biochar composite, and the results are shown in Table 1. The unmodified original biochar is used as a control for adsorbing the perfluorinated compounds in the water body under the same conditions. The adsorption amount of the perfluorocompound by the original biochar is shown in Table 1.
TABLE 1 adsorption removal Rate of different materials for perfluorocompounds in Water
| PFOS | PFOA | |
| Original biochar | 39.1％ | 40.7％ |
| Hydrophobic biochar composite material | 99.8％ | 98.6％ |
From the results of table 1, it can be seen that the adsorption capacity of the hydrophobic biochar composite material prepared in example 1 of the present invention to perfluoro compounds in an aqueous solution is significantly increased as compared to the original biochar. When the initial concentration of the perfluorinated compounds is 10mg/L, the adsorption and adsorption removal rate of the perfluorinated compounds in the water body by the hydrophobic biochar composite material is improved by more than 140% compared with that of the original biochar, which shows that the copolymer of the sulfobetaine and the acrylamide is modified on the surface of the biochar, so that the capability of the biochar for adsorbing hydrophobic pollutants is obviously enhanced.
The copolymer of the sulfobetaine and the acrylamide is used for modifying the biochar, so that the adsorption capacity of the adsorption material is improved, and the application of the biochar material in polluted water is expanded. The hydrophobic biochar composite material has the advantages of stable structure, strong adsorption capacity, high practical application value and the like, and is a novel biochar material with great prospect. The hydrophobic biochar composite material has remarkable adsorption and removal effects on hydrophobic pollutants in water, is suitable for repairing polluted water, has higher application value in the aspect of treating polluted water, and has wide application prospect.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (6)
1. The hydrophobic biochar composite material is characterized by comprising biochar, wherein the surface of the biochar is modified with a copolymer of sulfobetaine and acrylamide;
the preparation method of the hydrophobic biochar composite material comprises the following steps:
step one, preparing a mixed solution of acrylamide and [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide;
step two, putting the biochar into the mixed solution obtained in the step one to obtain black suspension;
step three, introducing nitrogen into the black suspension obtained in the step two for half an hour;
step four, adding ammonium persulfate and N, N, N, N-tetramethyl ethylenediamine into the black suspension obtained in the step three to react, so as to obtain a hydrophobic biochar composite material;
in the first step, the mass volume ratio of the acrylamide to the water in the mixed solution of the acrylamide and the [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide is 10 g-20 g:100mL of [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide and water, wherein the mass volume ratio of the [2- (methacryloyloxy) ethyl ] dimethyl- (3-sulfopropyl) ammonium hydroxide to water is 10-40 g:100mL;
in the second step, the mass volume ratio of the biochar to the mixed solution is 10-20 g:100mL; after mixing, stirring for 6-24 h at the temperature of 20-40 ℃ and the rotating speed of 160-180 rpm.
In the third step, 100-200 mL/min nitrogen is introduced into the mixed solution, and the mixed solution is stirred for 0.5-2 h at the temperature of 50-60 ℃ and the rotating speed of 120-180 rpm;
in the fourth step, the mass volume ratio of the ammonium persulfate to the black suspension is 2 mg-20 mg:100mL, wherein the mass volume ratio of the N, N, N, N-tetramethyl ethylenediamine to the black suspension is 5 g-20 g:100mL, wherein the reaction is carried out at 50-65 ℃ under stirring at a rotating speed of 100-180 rpm for 12h.
2. Use of the hydrophobic biochar composite according to claim 1 for adsorbing hydrophobic contaminants in a body of water.
3. The use of the hydrophobic biochar composite according to claim 2 for adsorbing hydrophobic contaminants in a body of water, wherein the use of the hydrophobic biochar composite for adsorbing hydrophobic contaminants in a body of water comprises: mixing the hydrophobic biochar composite material with a water body containing hydrophobic pollutants, and carrying out oscillation treatment to complete the adsorption treatment of the hydrophobic pollutants in the water body.
4. The use of the hydrophobic biochar composite according to claim 3 for adsorbing hydrophobic contaminants in a body of water, wherein the mass to volume ratio of the hydrophobic biochar composite to the body of water containing hydrophobic contaminants is between 0.1g and 1.0g:1L.
5. Use of a hydrophobic biochar composite according to claim 3 for adsorbing hydrophobic contaminants in a body of water, wherein the contaminants are perfluorinated compounds and the initial concentration of contaminants in the body of water containing contaminants is between 1mg/L and 100mg/L.
6. The use of the hydrophobic biochar composite according to claim 3, wherein the temperature of the shaking treatment is 20-35 ℃, the rotation speed of the shaking treatment is 150-200 rpm, and the time of the shaking treatment is 0.5-24 h.
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