CN115869979A - Preparation method of porous nitrogen-doped lignin biochar and application of porous nitrogen-doped lignin biochar in mediating reduction of hexavalent chromium - Google Patents
Preparation method of porous nitrogen-doped lignin biochar and application of porous nitrogen-doped lignin biochar in mediating reduction of hexavalent chromium Download PDFInfo
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- 229920005610 lignin Polymers 0.000 title claims abstract description 121
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000009467 reduction Effects 0.000 title claims description 15
- 239000000843 powder Substances 0.000 claims abstract description 136
- 238000000227 grinding Methods 0.000 claims abstract description 93
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 71
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000008367 deionised water Substances 0.000 claims abstract description 63
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 63
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 239000012298 atmosphere Substances 0.000 claims abstract description 13
- 125000001477 organic nitrogen group Chemical group 0.000 claims abstract description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 239000002351 wastewater Substances 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims description 90
- 238000001035 drying Methods 0.000 claims description 55
- 239000000706 filtrate Substances 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 35
- 230000007935 neutral effect Effects 0.000 claims description 35
- 238000005406 washing Methods 0.000 claims description 35
- 238000001816 cooling Methods 0.000 claims description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical group [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical group NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- 150000007529 inorganic bases Chemical class 0.000 claims description 3
- 125000005842 heteroatom Chemical group 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
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- 238000002474 experimental method Methods 0.000 abstract description 12
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- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 238000010000 carbonizing Methods 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 15
- 238000006722 reduction reaction Methods 0.000 description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- 239000012300 argon atmosphere Substances 0.000 description 11
- 238000000197 pyrolysis Methods 0.000 description 11
- 238000004088 simulation Methods 0.000 description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 239000011651 chromium Substances 0.000 description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 7
- 229910052804 chromium Inorganic materials 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 4
- 102000020897 Formins Human genes 0.000 description 4
- 108091022623 Formins Proteins 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
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- 235000019253 formic acid Nutrition 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 235000006408 oxalic acid Nutrition 0.000 description 4
- 230000008439 repair process Effects 0.000 description 4
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- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 2
- 239000001263 FEMA 3042 Substances 0.000 description 2
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229920002258 tannic acid Polymers 0.000 description 2
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 2
- 229940033123 tannic acid Drugs 0.000 description 2
- 235000015523 tannic acid Nutrition 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 125000004344 phenylpropyl group Chemical group 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
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- 229920001864 tannin Polymers 0.000 description 1
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- 239000001648 tannin Substances 0.000 description 1
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- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of composite materials, relates to lignin modification, and particularly relates to a preparation method of porous nitrogen-doped lignin biochar, which comprises the following steps: firstly, carbonizing and crushing lignin in an oxygen-insulating manner into powder, then uniformly mixing and stirring the lignin carbon powder, inorganic alkali or carbonate and deionized water according to a mass ratio of 3-6; pyrolyzing the mixture for 1.5 to 3.5 hours at the temperature of between 700 and 900 ℃ in an inert atmosphere, cleaning the mixture and grinding the mixture into powder; and mixing and stirring the porous lignin carbon powder, the organic nitrogen source and deionized water according to a mass ratio of 1-20. The invention adopts the environment-friendly process, has controllable process and simple and convenient operation, and does not generate secondary pollutants. The experiment simulates the hexavalent chromium in the catalytic reduction wastewater, the effect is excellent, the ultrahigh removal rate (> 99%) of 20mg/L hexavalent chromium can be reached within 15min at the fastest speed, and a referable theoretical model is provided for practical application.
Description
Technical Field
The invention belongs to the technical field of composite materials, relates to lignin modification, and particularly relates to a preparation method of porous nitrogen-doped lignin biochar and application of porous nitrogen-doped lignin biochar in mediated reduction of hexavalent chromium.
Background
Chromium in industrial wastewater is one of the toxic elements in the environment. Chromium exists in various oxidation states in water, and trivalent chromium and hexavalent chromium are main components. Hexavalent chromium, a typical heavy metal, has received much attention because of its high toxicity and wide sources. Research has confirmed that hexavalent chromium readily diffuses into water, is highly permeable to biological membranes, and can be converted into a range of intermediates that threaten human health. Therefore, the water body polluted by hexavalent chromium must be treated and discharged after reaching the national standard. Trivalent chromium, another oxidation state of chromium, has proven to be less toxic than hexavalent chromium and can be converted to Cr (OH) using lime or sodium hydroxide 3 The precipitate was easily removed from the water. Thus, the catalytic reduction of hexavalent chromium to trivalent chromium with low toxicity is an effective method for removing hexavalent chromium from water.
A method of removing chromium from a body of water comprising: physical adsorption, chemical or biological repair, and the like. In general, hexavalent chromium can be effectively removed in a physical adsorption process, but the selection of an adsorbent is crucial, and meanwhile, the regeneration of the adsorbent is also a big problem, so that the adsorbent cannot be popularized in practical application due to the fact that the adsorbent cannot be reused; the bioremediation process has the advantages of low operation cost and no secondary pollution, but the mechanism is not deeply researched at present and cannot be applied in a large scale; the chemical repair process refers to the reduction or fixation of hexavalent chromium by chemicals, often needs to consume a large amount of chemical agents which are easy to cause secondary pollution, such as sulfur dioxide, sodium bisulfite, ferrous sulfate, ferrous chloride and the like, and the traditional chemical repair method is greatly influenced by pH value, has strict technical requirements and high cost, and greatly limits the application of chemical repair.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to disclose a preparation method of porous nitrogen-doped lignin biochar, and the porous nitrogen-doped lignin biochar is applied to chemical remediation of hexavalent chromium pollution in a water body.
Technical scheme
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) The lignin powder is pyrolyzed for 1 to 2 hours at the temperature of 700 to 900 ℃ in inert atmosphere, and the heating rate is 5 to 10 ℃ per minute -1 Cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, drying, grinding and sieving to obtain 50-100 mesh lignin carbon powder;
b) Mixing and stirring uniformly lignin carbon powder, inorganic alkali or carbonate and deionized water according to a mass ratio of 3-6;
c) The obtained powder is pyrolyzed for 1.5 to 3.5 hours at the temperature of 700 to 900 ℃ in inert atmosphere, and the heating rate is 5 to 10 ℃ per minute -1 Cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, drying, grinding and sieving to obtain 50-100 mesh porous lignin carbon powder;
d) Mixing and stirring the porous lignin carbon powder, the organic nitrogen source and the deionized water uniformly according to a mass ratio of 1;
e) Pyrolyzing the powder in inert atmosphere at 700-900 deg.c for 1.5-3.5 hr at the rate of 5-10 deg.c/min -1 Cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, drying again, grinding and sieving to obtain 50-100 mesh porous nitrogen-doped lignin carbon powder.
In the preferred embodiment of the invention, the inert atmosphere in the steps a), c) and e) is nitrogen or argon.
In the preferred embodiment of the invention, the inorganic base in the step b) is sodium hydroxide or potassium hydroxide, preferably potassium hydroxide; the carbonate is potassium carbonate or sodium carbonate, preferably potassium carbonate.
In a preferred embodiment of the present invention, the organic nitrogen source in step d) is dicyandiamide, melamine, urea or 2-methylimidazole, preferably dicyandiamide.
In a preferred embodiment of the invention, the mass ratio of the porous lignin carbon powder, the organic nitrogen source and the deionized water in the step d) is 1.
According to the material prepared by the method, porous lignin carbon is used as a substrate, nitrogen atoms are doped with heteroatoms in the lignin carbon, the particle size is 10-25 mu m, and the surface of the biochar has a porous structure.
According to the invention, the lignin raw material is pyrolyzed at high temperature in an oxygen-limited environment to obtain amorphous biochar, and the pore expansion and nitrogen atom introduction of the biochar are realized by adopting a potassium salt melting method, a wet impregnation method and a pyrolysis carbonization method, so that the porous nitrogen-doped lignin biochar catalyst is successfully prepared. Because the lignin contains a large amount of phenylpropyl structures, the lignin is subjected to melting, agglomeration and deformation in the pyrolysis process, molecules are crosslinked into thermoplastic amorphous carbon, a porous structure is formed in the later preparation step under the etching action of potassium hydroxide, and the porous nitrogen-doped amorphous lignin carbon catalytic material is obtained after further nitrogen-rich organic matter impregnation and oxygen-limited carbonization treatment. The doping of nitrogen atoms not only changes the electron cloud distribution of the porous carbon material and forms more active sites to improve the catalytic performance of the porous carbon material, but also reduces the work function of the carbon material and improves the oxidation resistance of the carbon material.
The invention also aims to apply the prepared porous nitrogen-doped amorphous lignin carbon as a catalyst to mediate organic acid to reduce hexavalent chromium in wastewater.
And (3) experimental simulation: the porous nitrogen-doped amorphous lignin carbon prepared by the method is used as a catalyst, and organic acid (tannin, formic acid, acetic acid and oxalic acid) is selected to reduce hexavalent chromium, and the result shows that when the concentration of the hexavalent chromium is 20mg/L and the concentration of the organic acid is 5mM, 20mg of the catalyst is added into 50mL of solution, and the hexavalent chromium is completely reduced within 15min at the fastest speed.
The reagents used in the present invention are all commercially available.
The invention has the characteristics that:
(1) The prepared catalyst obtains larger specific surface area due to the etching effect of inorganic alkali/salt, and provides more catalytic active sites;
(2) According to the invention, a nitrogen atom is successfully used for replacing part of carbon atoms in a heterocyclic ring system by using an impregnation method, so that the electron cloud density is changed, the charge transfer efficiency is enhanced, and the capability of catalytic reduction of hexavalent chromium is obviously improved;
(3) The invention uses natural biomass, adopts an environment-friendly process, and has the advantages of low cost, high catalyst efficiency, excellent reusability and the like, thereby having wide application prospect.
Advantageous effects
The invention adopts an environment-friendly process, has controllable process and simple and convenient operation, and does not generate secondary pollutants. The aim of efficiently and quickly catalyzing and reducing hexavalent chromium is achieved by modifying the natural biomass lignin. The experiment simulates the hexavalent chromium in the catalytic reduction wastewater, the effect is excellent, the ultrahigh removal rate (> 99%) of 20mg/L hexavalent chromium can be reached within 15min at the fastest speed, and a referable theoretical model is provided for practical application.
Drawings
FIG. 1 is a scanning electron micrograph of the porous lignin carbon obtained in example 9 (wherein the left is 5000X times and the right is 20000X times).
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, heating at 700 ℃ for 1h under argon atmosphere, and heating at a temperature rise rate of 10 ℃ per minute -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, and washing with deionized water until the pH value of filtrate is inDrying, grinding and sieving to obtain lignin charcoal powder of 100 meshes;
b) Mixing the obtained lignin carbon powder, sodium hydroxide and deionized water in a mass ratio of 3:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in an argon atmosphere at a heating rate of 10 ℃ per minute -1 Keeping the temperature for 1h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after the mixture is cooled to room temperature, then washing the powder by deionized water until the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 100-mesh porous lignin carbon powder;
d) And (3) mixing the obtained porous lignin carbon powder, 2-methylimidazole and deionized water in a mass ratio of 1:5:500 for 8 hours, then drying, grinding and sieving to obtain 100 mesh powder;
e) Putting the powder obtained in the step d) into a tube furnace, and carrying out pyrolysis in the argon atmosphere at the temperature rise rate of 10 ℃ min -1 Keeping the temperature for 1h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after the mixture is cooled to room temperature, then washing the powder by deionized water until the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 50-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of tannic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 60 min.
Example 2
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, pyrolyzing for 1h at 700 ℃ under the atmosphere of argon gas, and heating up at a rate of 10 ℃ per minute -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, immediately drying, grinding and sieving to obtain 100 mesh lignin carbon powder;
b) Mixing the obtained lignin carbon powder, sodium hydroxide and deionized water in a mass ratio of 3:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in an argon atmosphere at a heating rate of 10 ℃ per minute -1 Keeping the temperature for 1h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after the mixture is cooled to room temperature, then washing the powder by deionized water until the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 100-mesh porous lignin carbon powder;
d) And (3) mixing the obtained porous lignin carbon powder, 2-methylimidazole and deionized water in a mass ratio of 1:20:500 stirring for 8h, then drying, grinding and sieving to obtain 100 mesh powder;
e) Putting the powder obtained in the step d) into a tubular furnace, and carrying out pyrolysis in an argon atmosphere at a heating rate of 10 ℃ per minute -1 Keeping the temperature for 1h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after the mixture is cooled to room temperature, then washing the powder by deionized water until the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 50-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of tannic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 60 min.
Example 3
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, pyrolyzing for 1h at 700 ℃ under the atmosphere of argon gas, and heating up at a rate of 10 ℃ per minute -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, immediately drying, grinding and sieving to obtain 100 mesh lignin carbon powder;
b) Mixing the obtained lignin carbon powder, sodium hydroxide and deionized water in a mass ratio of 6:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in an argon atmosphere at a heating rate of 10 ℃ per minute -1 Keeping for 1h after reaching 700 ℃, grinding and sieving to obtain 100-mesh powder after cooling to room temperature, then washing with deionized water until the filtrate is neutral, then drying, grinding and sieving to obtain 100-mesh porous powderLignin charcoal powder;
d) Mixing the obtained porous lignin carbon powder, 2-methylimidazole and deionized water in a mass ratio of 1:5:500 stirring for 8h, then drying, grinding and sieving to obtain 100 mesh powder;
e) Putting the powder obtained in the step d) into a tubular furnace, and carrying out pyrolysis in an argon atmosphere at a heating rate of 10 ℃ per minute -1 Keeping the temperature for 1h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after the mixture is cooled to room temperature, then washing the powder by deionized water until the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 50-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of formic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 45 min.
Example 4
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, pyrolyzing for 1.5h at 700 ℃ under the atmosphere of argon gas, and increasing the temperature rate at 10 ℃ per minute -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, immediately drying, grinding and sieving to obtain 100 mesh lignin carbon powder;
b) Mixing the obtained lignin carbon powder, sodium carbonate and deionized water according to a mass ratio of 3:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in an argon atmosphere at a heating rate of 10 ℃ min -1 Keeping the temperature for 1.5h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after the mixture is cooled to room temperature, then washing the powder by deionized water until the pH value of the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 100-mesh porous lignin carbon powder;
d) Mixing the obtained porous lignin carbon powder, urea and deionized water in a mass ratio of 1:5:500 stirring for 8h, then drying, grinding and sieving to obtain 100 mesh powder;
e) Placing the powder obtained in step d) in a tube furnacePyrolyzing in argon atmosphere at a heating rate of 10 ℃ for min -1 Keeping for 1.5h after reaching 700 ℃, cooling to room temperature, grinding and sieving to obtain 100-mesh powder, washing with deionized water until the pH of the filtrate is neutral, immediately drying, grinding and sieving to obtain 50-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of formic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 45 min.
Example 5
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, pyrolyzing for 1.5h at 700 ℃ under the atmosphere of argon gas, and increasing the temperature rate at 10 ℃ per minute -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, immediately drying, grinding and sieving to obtain 100 mesh lignin carbon powder;
b) Mixing the obtained lignin carbon powder, sodium carbonate and deionized water according to a mass ratio of 3:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in an argon atmosphere at a heating rate of 10 ℃ per minute -1 Keeping the temperature for 1.5h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after the mixture is cooled to room temperature, then washing the powder by deionized water until the pH value of the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 100-mesh porous lignin carbon powder;
d) Mixing the obtained porous lignin carbon powder, urea and deionized water in a mass ratio of 1:10:500 stirring for 8h, then drying, grinding and sieving to obtain 100 mesh powder;
e) Putting the powder obtained in the step d) into a tubular furnace, and carrying out pyrolysis in an argon atmosphere at a heating rate of 10 ℃ per minute -1 Keeping the temperature for 1.5h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after cooling to room temperature, then washing the powder by deionized water until the pH of the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 50-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of formic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 45 min.
Example 6
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, pyrolyzing for 1.5h at 700 ℃ under nitrogen atmosphere, and raising the temperature at 5 ℃ per minute -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100 mesh lignin carbon powder;
b) Mixing the obtained lignin carbon powder, sodium carbonate and deionized water according to a mass ratio of 3:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in a nitrogen atmosphere at a heating rate of 5 ℃ per minute -1 Keeping the temperature for 1.5h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after the mixture is cooled to room temperature, then washing the powder by deionized water until the pH value of the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 100-mesh porous lignin carbon powder;
d) And (3) mixing the obtained porous lignin carbon powder, urea and deionized water in a mass ratio of 1:15:500 for 8 hours, then drying, grinding and sieving to obtain 100 mesh powder;
e) Putting the powder obtained in the step d) into a tubular furnace, carrying out pyrolysis in nitrogen atmosphere, and heating at a rate of 5 ℃ for min -1 Keeping the temperature for 1.5h after the temperature reaches 700 ℃, grinding and sieving the mixture to obtain 100-mesh powder after the mixture is cooled to room temperature, then washing the powder by deionized water until the pH value of the filtrate is neutral, then drying the powder, and grinding and sieving the powder to obtain 100-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of acetic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 30 min.
Example 7
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, pyrolyzing for 2h at 700 ℃ under nitrogen atmosphere, and raising the temperature at a rate of 5 ℃ min -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100 mesh lignin carbon powder;
b) Mixing the obtained lignin carbon powder, potassium carbonate and deionized water in a mass ratio of 3:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in a nitrogen atmosphere at a heating rate of 5 ℃ per minute -1 Keeping for 2h after the temperature reaches 700 ℃, grinding and sieving to obtain 100-mesh powder after cooling to room temperature, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100-mesh porous lignin carbon powder;
d) Mixing the obtained porous lignin carbon powder, melamine and deionized water in a mass ratio of 1:20:500 stirring for 8h, then drying, grinding and sieving to obtain 100 mesh powder;
e) Putting the powder obtained in the step d) into a tubular furnace, and carrying out pyrolysis in nitrogen atmosphere at the temperature rise rate of 5 ℃ min -1 Keeping for 2h after the temperature reaches 700 ℃, grinding and sieving to obtain 100-mesh powder after cooling to room temperature, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of acetic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 20 min.
Example 8
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, pyrolyzing for 2h at 700 ℃ under nitrogen atmosphere, and raising the temperature at a rate of 5 ℃ per minute -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, and then removingWashing the seed water until the pH value of the filtrate is neutral, then drying, grinding and sieving to obtain lignin carbon powder of 100 meshes;
b) Mixing the obtained lignin carbon powder, potassium carbonate and deionized water in a mass ratio of 3:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in a nitrogen atmosphere at a heating rate of 5 ℃ per minute -1 Keeping for 2h after the temperature reaches 700 ℃, grinding and sieving to obtain 100-mesh powder after cooling to room temperature, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100-mesh porous lignin carbon powder;
d) And mixing the obtained porous lignin carbon powder, melamine and deionized water in a mass ratio of 1:20:500 for 8 hours, then drying, grinding and sieving to obtain 100 mesh powder;
e) Putting the powder obtained in the step d) into a tubular furnace, and carrying out pyrolysis in nitrogen atmosphere at the temperature rise rate of 5 ℃ min -1 Keeping for 2h after the temperature reaches 700 ℃, grinding and sieving to obtain 100-mesh powder after cooling to room temperature, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of oxalic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 15 min.
Example 9
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, pyrolyzing for 2h at 800 ℃ under nitrogen atmosphere, and raising the temperature at a rate of 5 ℃ per minute -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100 mesh lignin carbon powder;
b) Mixing the obtained lignin carbon powder, potassium hydroxide and deionized water in a mass ratio of 3:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in a nitrogen atmosphere at a heating rate of 5 ℃ per minute -1 Keeping for 2h after the temperature reaches 700 ℃, grinding and sieving to obtain 100-mesh powder after cooling to room temperature, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100-mesh porous lignin carbon powder;
d) And (3) mixing the obtained porous lignin carbon powder, dicyandiamide and deionized water in a mass ratio of 1:20:500 stirring for 8h, then drying, grinding and sieving to obtain 100 mesh powder;
e) Putting the powder obtained in the step d) into a tubular furnace, carrying out pyrolysis in nitrogen atmosphere, and heating at a rate of 5 ℃ for min -1 Keeping for 2h after the temperature reaches 700 ℃, grinding and sieving to obtain 100-mesh powder after cooling to room temperature, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of oxalic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 20 min.
Example 10
A preparation method of porous nitrogen-doped lignin biochar comprises the following steps:
a) Putting lignin powder into a tube furnace, pyrolyzing for 2h at 900 ℃ under nitrogen atmosphere, and raising the temperature at a rate of 5 ℃ per minute -1 After cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sieving to obtain 100 mesh lignin carbon powder;
b) And (3) mixing the obtained lignin carbon powder, potassium hydroxide and deionized water in a mass ratio of 3:1:200, mixing and stirring for 8 hours, then drying, grinding and sieving to obtain 100-mesh powder;
c) Putting the powder obtained in the step b) into a tube furnace, heating the powder in a nitrogen atmosphere at a heating rate of 5 ℃ per minute -1 Keeping for 2h after reaching 700 ℃, grinding and sieving to obtain 100 mesh powder after cooling to room temperature, then washing with deionized water until the pH of the filtrate is neutral, then drying, grinding and sievingObtaining 100-mesh porous lignin carbon powder;
d) And (3) mixing the obtained porous lignin carbon powder, dicyandiamide and deionized water in a mass ratio of 1:20:500 for 8 hours, then drying, grinding and sieving to obtain 100 mesh powder;
e) Putting the powder obtained in the step d) into a tubular furnace, carrying out pyrolysis in nitrogen atmosphere, and heating at a rate of 5 ℃ for min -1 Keeping for 2h after reaching 700 ℃, cooling to room temperature, grinding and sieving to obtain 100-mesh powder, then washing with deionized water until the pH of the filtrate is neutral, immediately drying, grinding and sieving to obtain 100-mesh porous nitrogen-doped lignin carbon powder.
Hexavalent chromium reduction experiment simulation: when the concentration of hexavalent chromium is 20mg/L and the concentration of oxalic acid is 5mM, 20mg of the catalyst prepared in the embodiment is added into 50mL of solution, and hexavalent chromium is completely reduced within 30 min.
The above description is only an embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications, equivalents, flow charts, and other related technical fields that are made by the present invention will be included in the scope of the present invention.
Claims (10)
1. A preparation method of porous nitrogen-doped lignin biochar is characterized by comprising the following steps:
a) The lignin powder is pyrolyzed for 1 to 2 hours at the temperature of 700 to 900 ℃ in inert atmosphere, and the heating rate is 5 to 10 ℃ per minute -1 Cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, drying, grinding and sieving to obtain 50-100 mesh lignin carbon powder;
b) Mixing and stirring uniformly lignin carbon powder, inorganic alkali or carbonate and deionized water according to a mass ratio of 3-6;
c) The obtained powder is pyrolyzed for 1.5 to 3.5 hours at the temperature of 700 to 900 ℃ in inert atmosphere, and the heating rate is 5 to 10 ℃ per minute -1 Cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, drying, grinding and sievingObtaining porous lignin carbon powder of 50-100 meshes;
d) Mixing and stirring the porous lignin carbon powder, the organic nitrogen source and the deionized water uniformly according to a mass ratio of 1;
e) Pyrolyzing the powder in inert atmosphere at 700-900 deg.c for 1.5-3.5 hr at the rate of 5-10 deg.c/min -1 Cooling to room temperature, grinding and sieving to obtain 50-100 mesh powder, washing with deionized water until the pH of the filtrate is neutral, drying again, grinding and sieving to obtain 50-100 mesh porous nitrogen-doped lignin carbon powder.
2. The method for preparing porous nitrogen-doped lignin biochar according to claim 1, wherein the method comprises the following steps: the inert atmosphere in step a), step c) and step e) is nitrogen or argon.
3. The method for preparing the porous nitrogen-doped lignin biochar according to claim 1, characterized in that: in the step b), the inorganic base is sodium hydroxide or potassium hydroxide, and the carbonate is potassium carbonate or sodium carbonate.
4. The method for preparing porous nitrogen-doped lignin biochar according to claim 3, wherein the method comprises the following steps: in the step b), the inorganic base is potassium hydroxide, and the carbonate is potassium carbonate.
5. The method for preparing the porous nitrogen-doped lignin biochar according to claim 1, characterized in that: in the step d), the organic nitrogen source is dicyandiamide, melamine, urea or 2-methylimidazole.
6. The method for preparing porous nitrogen-doped lignin biochar according to claim 5, wherein the method comprises the following steps: the organic nitrogen source in the step d) is dicyandiamide.
7. The method for preparing porous nitrogen-doped lignin biochar according to claim 1, wherein the method comprises the following steps: and d) uniformly mixing and stirring the porous lignin carbon powder, the organic nitrogen source and the deionized water according to the mass ratio of 1.
8. The porous nitrogen-doped lignin biochar prepared according to any one of claims 1-7.
9. The porous nitrogen-doped lignin biochar of claim 8, wherein: the porous lignin carbon is used as a substrate, nitrogen atoms are doped with heteroatoms in the porous lignin carbon, the particle size is 10-25 mu m, and the surface of the biochar has a porous structure.
10. Use of the porous nitrogen-doped lignin biochar according to claim 8 or 9, wherein: the catalyst is used as a catalyst to mediate hexavalent chromium in organic acid reduction wastewater.
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