CN111514854A - Preparation method of modified 3D porous carbon composite adsorption material - Google Patents
Preparation method of modified 3D porous carbon composite adsorption material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000002131 composite material Substances 0.000 title claims abstract description 65
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 62
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 3
- 159000000009 barium salts Chemical class 0.000 claims abstract description 3
- 150000001621 bismuth Chemical class 0.000 claims abstract description 3
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 3
- 239000001103 potassium chloride Substances 0.000 claims abstract description 3
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 7
- 235000010333 potassium nitrate Nutrition 0.000 claims description 7
- 239000004323 potassium nitrate Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 5
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 5
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 5
- 239000011425 bamboo Substances 0.000 claims description 5
- -1 K in BaO2O Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 3
- 244000060011 Cocos nucifera Species 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 244000082204 Phyllostachys viridis Species 0.000 claims 1
- 239000003463 adsorbent Substances 0.000 abstract description 12
- 150000002500 ions Chemical class 0.000 abstract description 12
- 239000000203 mixture Substances 0.000 abstract description 11
- 238000012986 modification Methods 0.000 abstract description 6
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 3
- 239000012876 carrier material Substances 0.000 abstract description 2
- 239000000945 filler Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 6
- 241001330002 Bambuseae Species 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- 230000004913 activation Effects 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000005287 template synthesis Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 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
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—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 form
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- 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
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- 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
- C02F2101/20—Heavy metals or heavy metal compounds
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
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Abstract
A preparation method of a modified 3D porous carbon composite adsorption material relates to the technical field of composite modification for preparing an activated carbon adsorption material, and comprises the steps of dissolving sylvite, barium salt and bismuth salt in water, uniformly mixing, adding activated carbon, uniformly mixing, and reacting through an ultrasonic microwave combined reactor to prepare the modified 3D porous carbon composite adsorption material. The invention takes 3D porous carbon as a main carrier material and K with certain content and composition2O‑Bi2O3-BaO is used as filler of adsorbing material, and composite adsorbing material with excellent performance is prepared by newly developed ultrasonic and microwave combined methodAnd (3) attaching materials. At the same time, doping K with different molar ratios2O‑Bi2O3Modification research is carried out on the porous carbon adsorption material by BaO substance ions. The better composite 3D porous carbon component adsorbent material is obtained. The series porous carbon composite materials with different compositions have different adsorption capacity, removal time and material composition on the heavy metal ion solution containing Pb (II) ions.
Description
Technical Field
The invention relates to the technical field of preparation of an activated carbon adsorption material by composite modification, and particularly relates to a preparation method of a modified 3D porous carbon composite adsorption material.
Background
In recent years, with the rapid development of economy and science and technology, a porous carbon material is a pollution-free and environment-friendly adsorbent material. A large number of experiments and researches show that the composite porous carbon material has better adsorption and catalysis performances than a single porous carbon material due to the unique performance of the composite porous carbon material. The porous carbon composite adsorption material has rich porous structure, ultrahigh specific surface area and rich surface functional groups, and is widely applied to the fields of adsorption separation, sewage treatment, gas purification and the like.
The 3D porous carbon material has a unique framework structure, a high surface area, directional pore channel distribution, high chemical stability and a strong double electric layer effect, is widely paid attention to at present due to a unique three-dimensional structure, and can be used as a carbon electrode material of lithium batteries, lithium sulfur and super capacitors by loading a certain amount of metal compounds.
Common synthesis methods of the 3D porous carbon material include a carbonization method, a physicochemical activation method, a catalytic activation method, an organogel carbonization method, a self-assembly method, a template method and the like. The metal of the catalytic activation method is easy to enter and stay in the porous carbon, the organic gel carbonization method is expensive and complicated in preparation process, and the precursor of the organic aerogel uses toxic organic matters such as phenol and aldehyde, so that the organic aerogel has certain danger to workers and the environment. The template synthesis process of the traditional template method is complicated, the cost is high and the like, so that the large-scale application of the template in industrial production is limited.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a modified 3D porous carbon composite adsorption material to prepare the adsorption material which can be used for treating industrial sewage and wastewater environment containing lead ions.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a modified 3D porous carbon composite adsorption material comprises the steps of dissolving sylvite, barium salt and bismuth salt in water, uniformly mixing, adding activated carbon, uniformly mixing, reacting through an ultrasonic microwave combined reactor, and preparing to obtain the modified 3D porous carbon composite adsorption material C-K2O-Bi2O3-BaO。
As a preferred technical scheme of the preparation method of the modified 3D porous carbon composite adsorption material, the preparation method comprises the following specific steps:
1) weighing potassium nitrate, barium nitrate and bismuth nitrate, adding into a beaker, dissolving with distilled water, adding ammonia water under magnetic stirring to adjust the pH value of the solution to 9-12, and adjusting the pH value with the ammonia water solution after fully stirring;
2) ball-milling the activated carbon powder into fine powder with the particle size of 1-5 mu m, adding the fine powder into the solution, fully stirring, and adjusting the pH value of the solution to 9-12 by using an ammonia water solution;
3) putting the solution into an ultrasonic and microwave combined reactor for reaction, and carrying out double-functional reaction for 30min by adopting ultrasonic waves 1200W and microwaves 1000W;
4) after the reaction is finished, putting the sample into a drying oven at 150 ℃ for drying for 6 hours to obtain the modified 3D porous carbon composite adsorption material C-K2O-Bi2O3-BaO。
As modified 3D porous carbon composite adsorbent material of the present inventionAccording to a further preferable technical scheme of the preparation method, the activated carbon is selected from one of coal activated carbon powder, bamboo activated carbon powder and coconut shell activated carbon powder. Modified 3D porous carbon composite adsorption material C-K2O-Bi2O3C, K in BaO2O、Bi2O3And the doping molar ratio of BaO is 5-10: 1-5: 1-5: 1 to 5. Further preferably, the modified 3D porous carbon composite adsorption material C-K2O-Bi2O3C, K in BaO2O、Bi2O3And the doping molar ratio of BaO is 7: 1: 2: 1.
the invention provides a modified 3D porous carbon composite adsorption material C-K2O-Bi2O3BaO, the microscopic form is a porous structure composed of shapes of a sheet, a rod, a tetrahedron and the like, and the microstructure size range of the composite material is 500nm-2 um.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes the prepared 3D porous carbon as a main carrier material and K with certain content and composition2O-Bi2O3BaO is used as a filler of the adsorption material, and a composite adsorption material with excellent performance is prepared by a newly developed ultrasonic and microwave combined method. At the same time, doping K with different molar ratios2O-Bi2O3Modification research is carried out on the porous carbon adsorption material by BaO substance ions. The modified porous carbon composite adsorption material is characterized by means such as XRD, SEM and the like. Through the comparison of the microstructure and the components, a better series of modified porous carbon composite adsorption materials are selected, and the adsorption performance of the materials is researched and analyzed, so that a better composite 3D porous carbon component adsorbent material is obtained. Experiments show that the adsorption capacity, the removal time and the material composition of the series porous carbon composite materials with different compositions to the heavy metal ion solution containing Pb (II) ions are different. As a result, it was found that K2O-Bi2O3The adsorption effect of the-BaO (1: 2: 1) modified 3D porous carbon (70%) is the best, and the adsorption quantity reaches 239 mg/g. The target products prepared achieved the expected goals of the design of the experiment, these K's are expected2O-Bi2O3-BaO modified 3D porous carbon adsorptionThe material can be used for the environmental treatment of industrial sewage and wastewater containing lead ions.
Drawings
The following provides further details of the preparation method of the modified 3D porous carbon composite adsorption material according to the present invention with reference to examples and drawings.
FIG. 1 is an XRD pattern of each series of composite adsorbents prepared in examples 1 to 10.
Fig. 2 is SEM images of low, medium, and high magnification in order of the composite adsorbent prepared in example 1.
FIG. 3 is a graph showing percentage of lead ions remaining in the adsorption of each series of composite adsorbent materials prepared in examples 1 to 7.
FIG. 4 is a graph showing the adsorption amount of each series of composite adsorbents prepared in examples 1 to 7.
Detailed Description
Example 1
In the implementation, the prepared modified 3D porous carbon composite adsorbing material C-K2O-Bi2O3in-BaO, C, K2O、Bi2O3And the doping molar ratio of BaO is 7: 1: 2: 1. the preparation method comprises the following steps:
1) weighing potassium nitrate, barium nitrate and bismuth nitrate according to a molar ratio, adding the potassium nitrate, the barium nitrate and the bismuth nitrate into a beaker, dissolving the potassium nitrate, the barium nitrate and the bismuth nitrate by using distilled water, adding ammonia water under magnetic stirring to adjust the pH value of the solution to 12, and adjusting the pH value of the solution by using the ammonia water solution after fully stirring.
2) Ball-milling the bamboo wood activated carbon powder into fine powder with the particle size of 1 mu m, adding the fine powder into the solution, fully stirring the solution, and adjusting the pH value of the solution to 12 by using an ammonia water solution.
3) And placing the solution in an ultrasonic and microwave combined reactor for reaction, and performing double-functional reaction for 30min by adopting ultrasonic waves 1200W and microwaves 1000W.
4) After the reaction is finished, putting the sample into a drying oven at 150 ℃ for drying for 6 hours to obtain the modified 3D porous carbon composite adsorption material C-K2O-Bi2O3-BaO(7-1-2-1)。
Example 2
In this example, the prepared modified 3D porous carbon composite adsorbing material C-K2O-Bi2O3in-BaO, C, K2O、Bi2O3And the doping molar ratio of BaO is 7: 1: 1: 1, the preparation method is the same as that of example 1, and the modified 3D porous carbon composite adsorption material C-K is obtained2O-Bi2O3-BaO(7-1-1-1)。
Example 3
In this example, the prepared modified 3D porous carbon composite adsorbing material C-K2O-Bi2O3in-BaO, C, K2O、Bi2O3And the doping molar ratio of BaO is 7: 1: 1: 2, the preparation method is the same as that of example 1, and the modified 3D porous carbon composite adsorbing material C-K is obtained2O-Bi2O3-BaO(7-1-1-2)。
Example 4
In this example, the prepared modified 3D porous carbon composite adsorbing material C-K2O-Bi2O3in-BaO, C, K2O、Bi2O3And the doping molar ratio of BaO is 7: 1: 2: 2, the preparation method is the same as that of example 1, and the modified 3D porous carbon composite adsorbing material C-K is obtained2O-Bi2O3-BaO(7-1-2-2)。
Example 5
In this example, the prepared modified 3D porous carbon composite adsorbing material C-K2O-Bi2O3in-BaO, C, K2O、Bi2O3And the doping molar ratio of BaO is 7: 2: 1: 1, the preparation method is the same as that of example 1, and the modified 3D porous carbon composite adsorption material C-K is obtained2O-Bi2O3-BaO(7-2-1-1)。
Example 6
In this example, the prepared modified 3D porous carbon composite adsorbing material C-K2O-Bi2O3in-BaO, C, K2O、Bi2O3And the doping molar ratio of BaO is 7: 2: 1: 2, the preparation method is the same as that of example 1, and the modified 3D porous carbon composite adsorbing material C-K is obtained2O-Bi2O3-BaO(7-2-1-2)。
Example 7
In this example, modification 3 was obtainedD porous carbon composite adsorption material C-K2O-Bi2O3in-BaO, C, K2O、Bi2O3And the doping molar ratio of BaO is 7: 2: 2: 1, the preparation method is the same as that of example 1, and the modified 3D porous carbon composite adsorption material C-K is obtained2O-Bi2O3-BaO(7-2-2-1)。
Example 8
In this example, only Bi is doped2O3The raw materials do not contain potassium nitrate, barium nitrate, C and Bi2O3Is 7: 3, the other steps are the same as the example 1, and the modified 3D porous carbon composite adsorbing material C-Bi is obtained2O3(7-3)。
Example 9
In this example, only BaO was doped, the raw materials for preparation did not contain potassium nitrate and bismuth nitrate, and the doping molar ratio of C to BaO was 7: 3, the other steps are the same as the example 1, and the modified 3D porous carbon composite adsorbing material C-BaO (7-3) is obtained.
Example 10
In this example, only K was doped2O, barium nitrate, bismuth nitrate, C and K are not contained in the preparation raw materials2The doping molar ratio of O is 7: 3, obtaining the modified 3D porous carbon composite adsorption material C-K in the same way as the example 1 in other steps2O(7-3)。
FIG. 1 is an XRD pattern of each series of composite adsorbents prepared in examples 1 to 10. As can be seen from FIG. 1, the diffraction intensity peak and C-K of the sample2O-Bi2O3The phases of-BaO are basically corresponding, the positions of diffraction peaks of the series diffraction spectrograms are basically consistent, the peak intensity ratio has obvious difference, and the XRD diffraction pattern has obvious Bi2O3，BaO，K2The diffraction peaks of O are relatively sharp, which indicates that the synthesized composite adsorbent is in phase with the experimental design target 3D porous C-K2O-Bi2O3BaO fit.
Fig. 2 is SEM images of low, medium, and high magnification in order of the composite adsorbent prepared in example 1. As can be seen from FIG. 2, the modified 3D porous carbon composite adsorbent C-K obtained in the present example2O-Bi2O3-BaO(7-1-2-1)The composite material is a porous structure formed by shapes such as a sheet shape, a rod shape, a tetrahedron shape and the like, and the size range of the microstructure of the composite material is 500nm-2 um.
FIG. 3 shows the influence of the preparation of porous carbon composite materials of different compositions in examples 1 to 7 on the removal rate of a Pb (II) -ion-containing heavy metal ion solution under a sunlight condition. The dosage of the modified 3D porous carbon adsorption material is 30mg, the adsorption time is 150min, the volume of the Pb (II) solution is 100mL, and the initial concentration is 100 mg/L. As can be seen from FIG. 3, example 1 produces C-K2O-Bi2O3The best adsorption effect of the-BaO (7-1-2-1) is achieved, the removal rate reaches 99.8%, and the better adsorption removal effect is achieved when all series products with different compositions are prolonged along with time.
FIG. 4 is a curve of adsorption capacity, removal time and substance composition of a Pb (II) -ion-containing heavy metal ion solution of a series of porous carbon composite materials with different compositions prepared in examples 1 to 7 under a sunlight condition. The dosage of the modified 3D porous carbon adsorption material is 50mg, the adsorption time is 140min, and the volume of the Pb (II) solution is 500 mL. As can be seen from FIG. 4, example 1 produces C-K2O-Bi2O3The best adsorption effect of the-BaO (7-1-2-1) is achieved, the adsorption amount reaches 239mg/g, and the adsorption removal effect of all series products with different compositions is better along with the prolonging of time. Meanwhile, it can be seen that the adsorption amount is basically stable with the increase of time after the adsorption time reaches 60 minutes, which indicates that the adsorption process is mainly completed within 60 minutes and the adsorption effect is good. Therefore, the C-K prepared by the invention is proved by experiments2O-Bi2O3the-BaO modified 3D porous carbon adsorption material can be used for environmental treatment of industrial sewage and wastewater containing lead ions.
Example 11
In this example, ammonia was added to adjust the pH to 10, and the other steps were the same as in example 1.
Example 12
In this example, bamboo activated carbon was replaced with coal activated carbon powder, and the other steps were the same as in example 1.
Example 13
In this example, bamboo and wood activated carbon was replaced with coconut shell activated carbon powder, and the particles were ball-milled uniformly to 5 μm fine powder, and the other steps were the same as in example 1.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (6)
1. A preparation method of a modified 3D porous carbon composite adsorption material is characterized by firstly dissolving sylvite, barium salt and bismuth salt in water, uniformly mixing, then adding activated carbon, uniformly mixing, and then reacting through an ultrasonic microwave combined reactor to prepare the modified 3D porous carbon composite adsorption material C-K2O-Bi2O3-BaO。
2. The preparation method according to claim 1, comprising the following steps:
1) weighing potassium nitrate, barium nitrate and bismuth nitrate, adding into a beaker, dissolving with distilled water, adding ammonia water under magnetic stirring to adjust the pH value of the solution to 9-12, and adjusting the pH value with the ammonia water solution after fully stirring;
2) ball-milling the activated carbon powder into fine powder with the particle size of 1-5 mu m, adding the fine powder into the solution, fully stirring, and adjusting the pH value of the solution to 9-12 by using an ammonia water solution;
3) putting the solution into an ultrasonic and microwave combined reactor for reaction, and carrying out double-functional reaction for 30min by adopting ultrasonic waves 1200W and microwaves 1000W;
4) after the reaction is finished, putting the sample into a drying oven at 150 ℃ for drying for 6 hours to obtain the modified 3D porous carbon composite adsorption material C-K2O-Bi2O3-BaO。
3. The method of claim 1 or 2, wherein the activated carbon is selected from one of coal activated carbon powder, bamboo activated carbon powder, and coconut shell activated carbon powder.
4. The preparation method according to claim 2, wherein the modified 3D porous carbon composite adsorption material C-K2O-Bi2O3C, K in BaO2O、Bi2O3And the doping molar ratio of BaO is 5-10: 1-5: 1-5: 1 to 5.
5. The preparation method according to claim 4, wherein the modified 3D porous carbon composite adsorption material C-K2O-Bi2O3C, K in BaO2O、Bi2O3And the doping molar ratio of BaO is 7: 1: 2: 1.
6. the modified 3D porous carbon composite adsorption material C-K prepared by the method of any one of claims 1 to 52O-Bi2O3BaO, characterized in that the microscopic morphology is a porous structure composed of sheet, rod, tetrahedron, etc., and the microstructure size of the composite material is in the range of 500nm-2 um.
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