CN113941314B - Seawater modified biochar and preparation method and application thereof - Google Patents
Seawater modified biochar and preparation method and application thereof Download PDFInfo
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- 239000013535 sea water Substances 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 100
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 100
- 239000011574 phosphorus Substances 0.000 claims abstract description 100
- 239000000203 mixture Substances 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 37
- 239000002028 Biomass Substances 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 238000000227 grinding Methods 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000000197 pyrolysis Methods 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 66
- 108010059993 Vancomycin Proteins 0.000 claims description 21
- 229960003165 vancomycin Drugs 0.000 claims description 21
- MYPYJXKWCTUITO-LYRMYLQWSA-N vancomycin Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C2C=C3C=C1OC1=CC=C(C=C1Cl)[C@@H](O)[C@H](C(N[C@@H](CC(N)=O)C(=O)N[C@H]3C(=O)N[C@H]1C(=O)N[C@H](C(N[C@@H](C3=CC(O)=CC(O)=C3C=3C(O)=CC=C1C=3)C(O)=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)O2)=O)NC(=O)[C@@H](CC(C)C)NC)[C@H]1C[C@](C)(N)[C@H](O)[C@H](C)O1 MYPYJXKWCTUITO-LYRMYLQWSA-N 0.000 claims description 21
- MYPYJXKWCTUITO-UHFFFAOYSA-N vancomycin Natural products O1C(C(=C2)Cl)=CC=C2C(O)C(C(NC(C2=CC(O)=CC(O)=C2C=2C(O)=CC=C3C=2)C(O)=O)=O)NC(=O)C3NC(=O)C2NC(=O)C(CC(N)=O)NC(=O)C(NC(=O)C(CC(C)C)NC)C(O)C(C=C3Cl)=CC=C3OC3=CC2=CC1=C3OC1OC(CO)C(O)C(O)C1OC1CC(C)(N)C(O)C(C)O1 MYPYJXKWCTUITO-UHFFFAOYSA-N 0.000 claims description 21
- 241000233866 Fungi Species 0.000 claims description 18
- 240000008042 Zea mays Species 0.000 claims description 16
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 16
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 16
- 235000005822 corn Nutrition 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 230000001105 regulatory effect Effects 0.000 claims description 12
- 239000012535 impurity Substances 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 8
- 239000002699 waste material Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 230000003115 biocidal effect Effects 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000002064 nanoplatelet Substances 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 30
- 238000012986 modification Methods 0.000 abstract description 12
- 230000004048 modification Effects 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 11
- 238000012851 eutrophication Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 description 53
- 239000003463 adsorbent Substances 0.000 description 23
- 239000003610 charcoal Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 18
- 239000011777 magnesium Substances 0.000 description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 12
- 239000011575 calcium Substances 0.000 description 12
- 229910052749 magnesium Inorganic materials 0.000 description 12
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 11
- 229910052791 calcium Inorganic materials 0.000 description 11
- 239000000706 filtrate Substances 0.000 description 8
- 230000007935 neutral effect Effects 0.000 description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000002715 modification method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 230000007613 environmental effect Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 235000020774 essential nutrients Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- -1 phosphate anions Chemical class 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010907 stover Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
-
- 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
-
- 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
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4893—Residues derived from used synthetic products, e.g. rubber from used tyres
-
- 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
- C02F2101/105—Phosphorus compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses seawater modified biochar and a preparation method and application thereof. The preparation method of the seawater modified biochar comprises the following steps: washing, airing, crushing and grinding biomass to obtain biomass powder; filtering natural seawater; preparing biomass powder into biochar by adopting a pyrolysis method or a hydrothermal method; mixing biochar and filtered seawater according to a certain proportion, stirring, then dropwise adding alkali liquor into the mixture to adjust the pH value of the mixture to 10-11, continuing stirring, and standing the mixture for constant-temperature aging; filtering the aged mixture, collecting solids, washing the solids, drying, grinding and sieving to obtain the seawater modified biochar. The seawater modified biochar provided by the invention is low in preparation cost, has excellent adsorption capacity on phosphorus in water, can effectively solve the problems of high preparation cost and poor modification effect of the current modified biochar, and provides a new way for water eutrophication treatment.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to seawater modified biochar and a preparation method and application thereof.
Background
Phosphorus is an important chemical raw material and is an essential nutrient element in the growth process of animals and plants. Currently, 90% of the worldwide phosphorus is derived from phosphate ores. If the phosphate rock is used up as a non-renewable resource within 100 years at the current consumption rate. As can be seen, the world is faced with a situation where phosphorus resources are scarce. However, in industrial production and large-scale agricultural development, a large amount of phosphorus is not fully utilized and is discharged into water. When the phosphorus concentration in the water body is too high, the water body can be eutrophicated, algae and plankton are greatly propagated, and the concentration of dissolved oxygen in the water is greatly reduced, so that the environmental problems of death of fish and shrimp, black and odorous water body and the like are caused. Therefore, the phosphorus is recovered from the polluted water body, so that the phosphorus pollution of the water body can be effectively controlled, and the situation of shortage of global phosphorus resources can be relieved.
Biochar is a carbon-rich material and is prepared from biomass through high-temperature oxygen-limited pyrolysis or low-temperature hydrothermal carbonization. In recent years, biochar has been attracting attention because of its special properties and wide range of uses. At present, expert scholars have explored the application of biochar in the fields of agricultural production, farmland management, livestock and poultry aquatic production, carbon fixation, emission reduction, pollution control and the like. Generally, biochar has a larger comparison area, and the surface of the biochar is rich in a large amount of functional groups, so that the biochar is considered as a potential adsorbing material and can be used for adsorbing various pollutants in water bodies, such as heavy metals (such as copper, cadmium, lead, zinc and the like), nutrient elements (nitrogen, phosphorus) and emerging organic pollutants (such as antibiotics, bactericides and the like). Among them, adsorption of phosphorus in a water body by biochar has become a research hot spot. Biochar itself has the effect of improving soil, and phosphorus is a necessary nutrient for plant growth. Therefore, the biochar adsorbed with phosphorus can be applied to soil to further improve the soil fertility and realize the recycling of phosphorus resources. In general, most freshly prepared biochar surfaces are negatively charged, repel phosphate anions in water, and have a relatively low adsorption capacity for phosphorus. Therefore, how to improve the adsorption capacity of the biochar to phosphorus in water is a scientific problem which needs to be solved currently.
The biochar modification technology is one way to improve the adsorption capacity of biochar, and can improve the adsorption capacity of biochar. The most studied modification method currently is to load a metal element having a higher affinity for phosphorus onto the surface of biochar. These metals include calcium, magnesium, zinc, lanthanum, cerium, and the like. Chinese patent application No. 201910410211.5 discloses a high-efficiency dephosphorization biochar, which is loaded with lanthanum, and has a good effect of adsorbing phosphorus, but the lanthanum is a rare earth metal, so that resources are rare and the cost is high. Chinese patent application No. 202110777545.3 proposes a preparation method of a supported sludge-based biomass charcoal adsorbent, which uses aluminum and zinc to modify biochar, but the prepared biochar has the risk of zinc leaching when being used for water purification, and is easy to cause secondary pollution of water.
In contrast, calcium and magnesium are abundant in the crust, and are nontoxic in the water body, so that the calcium and magnesium are metal elements most suitable for modifying biochar. However, the methods for preparing the calcium/magnesium modified biochar reported so far all use high-concentration calcium/magnesium chemical reagents (such as CaCl 2 And MgCl 2 ) Resulting in high biochar production costs. In addition, the adsorption capacity of the modified biochar prepared by utilizing calcium/magnesium modification to phosphorus is still not high. For example, cui et al use MgCl at a concentration of 1.0mol/L 2 The solution was used to modify wetland plant biochar with a maximum adsorption capacity for phosphorus of only 27.63mg/g (Cui et al,Bioresource Technology2016, 218:1123-1132); jung et al uses MgCl at a concentration of up to 27mol/L 2 The solution produced magnesium modified biochar with a maximum adsorption capacity for phosphorus of only 16.10mg/g (Jung et al,Bioresource Technology, 2016, 200: 1029-1032). Therefore, the current method for modifying the biochar has the defects of high preparation cost and poor modification effect, and greatly limits the large-scale preparation and application of the modified biochar. If the modified biochar with high phosphorus adsorption performance can be prepared by using a low-cost calcium/magnesium source, the preparation cost of the modified biochar is greatly reduced, and the industrialized application of the modified biochar in the fields of pollution control and water purification is promoted.
Disclosure of Invention
In order to solve the defects and the shortcomings of the prior art, the invention aims to provide seawater modified biochar and a preparation method and application thereof. The method takes seawater as a cheap calcium/magnesium source to modify the biochar, has the characteristics of simple operation, easily available raw materials, low manufacturing cost, good modification effect and easy mass production, can effectively solve the problems of high preparation cost and poor modification effect in the existing biochar modification method, and provides a new way for eutrophication of water bodies and recovery of phosphorus in sewage in China.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of seawater modified biochar, which comprises the following steps:
(1) Cleaning, airing, crushing and grinding biomass to obtain biomass powder for later use;
(2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
(3) Preparing biochar by adopting a pyrolysis method or a hydrothermal method;
(4) Mixing biochar and filtered seawater according to the proportion of 0.2-3:1000 w/v, stirring, then adding alkali liquor dropwise into the mixture to adjust the pH value of the biochar/seawater mixture to 10-11, continuing stirring, and standing the mixture for constant-temperature aging;
(5) Filtering the aged mixture, collecting solids, washing the solids, drying, grinding and sieving to obtain the seawater modified biochar.
In the step (1), the biomass is any one of agricultural and forestry waste and antibiotic residues.
Furthermore, the agricultural and forestry waste is any one of fir branches and corn stalks, and the antibiotic fungus residues are vancomycin fungus residues with the water content of 60-70%.
Further, in the step (3), the pyrolysis method is as follows: and (3) placing the biomass powder in a crucible, placing the crucible in a muffle furnace, starting heating, and raising the temperature from room temperature to 600 ℃, keeping the temperature for 2 hours at a heating rate of 10 ℃/min, so that the biomass powder is pyrolyzed to biochar at a high temperature. The inventor experiment comparison shows that the specific area of the biochar prepared under the condition is the largest.
Further, in the step (3), the hydrothermal method is: and (3) taking pure water as a solvent, wherein the filling degree is 50%, putting 3-5 g of biomass powder into a hydrothermal reaction kettle, adding 50mL of pure water, adjusting the temperature to 140-220 ℃, and keeping the temperature for 15h to enable the biomass powder to be carbonized into biochar in a hydrothermal manner.
Further, in the step (4), the alkali liquor is a NaOH solution with the concentration of 1-3 mol/L.
Further, in the step (4), the ratio of the biochar to the seawater is preferably 2:1000w/v. The ratio can ensure the modification effect and reduce the use amount of seawater.
Further, in step (4), the pH of the mixture is adjusted to 10.50. The ratio modification effect is better, and meanwhile, the dosage of NaOH solution is less.
Further, in the step (4), the aging condition is 30-80 ℃ for 8-16 hours.
Further, in the step (5), the drying temperature is 60-105 ℃.
The invention also provides the seawater modified biochar prepared by the preparation method.
The invention also provides application of the seawater modified biochar in phosphorus adsorption.
The invention has the beneficial effects that:
compared with the prior art, the preparation method of the seawater modified biochar has the characteristics of easily available raw materials, simple operation, low manufacturing cost, good modification effect and easiness in large-scale production, and can effectively solve the problems of high preparation cost and poor modification effect of the conventional biochar modification method. In addition, the seawater modified biochar can effectively adsorb phosphorus in water, has high adsorption capacity, and can provide reference for efficient treatment of sewage with exceeding phosphorus standard. Meanwhile, the invention utilizes waste fir branches, corn stalks and vancomycin fungus residues as biomass raw materials, so that the waste biomass can be fully utilized, and the invention is a sewage treatment technology for treating waste by waste. In addition, the invention uses the seawater as the cheap calcium/magnesium source to modify the biochar, fully utilizes the calcium/magnesium resources contained in the seawater, and can provide a new way for the development and utilization of the seawater resources.
Drawings
FIG. 1 is a scanning electron microscope image of fir charcoal prepared in comparative example 1.
FIG. 2 is a scanning electron microscope image of the seawater-modified biochar prepared in example 1.
Detailed Description
The invention will be further illustrated with reference to specific examples. The examples of the present invention are intended to provide a better understanding of the present invention to those skilled in the art, and are not intended to limit the present invention in any way. The methods are conventional methods unless otherwise specified, and the starting materials are commercially available from the public sources unless otherwise specified.
Example 1
The preparation method of the seawater modified biochar comprises the following steps:
(1) Cleaning fir tree branches, airing, crushing and grinding to obtain fir tree branch powder for later use;
(2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
(3) Putting fir branch powder into a crucible, wrapping tin foil paper on a crucible opening, covering a crucible cover, putting into a muffle furnace, starting heating, and keeping the temperature from room temperature to 600 ℃ for 2 hours at a heating rate of 10 ℃/min to enable the fir branch powder to be pyrolyzed into fir biochar;
(4) Mixing 2g of fir charcoal with 1L of filtered seawater, stirring at 250rpm for 1h, then dropwise adding 1mol/L NaOH solution into the mixture to adjust the pH value of the fir charcoal/seawater mixture to 10.50, continuing stirring for 1h, and standing the mixture at 40 ℃ for constant temperature aging for 12h;
(5) Filtering the aged mixture, collecting solid, washing the solid with pure water until the filtrate is neutral, drying at 80 ℃, grinding and sieving to obtain the seawater modified biochar.
The seawater modified biochar prepared in the embodiment is used as an adsorbent for treating the phosphorus-containing wastewater with the phosphorus concentration of 98.5 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 3.0 by HCl or NaOH, 0.5g of adsorbent is added into 1L of the phosphorus-containing wastewater, and the mixture is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 26.0mg/L, and the adsorption capacity of the seawater modified biochar prepared in the embodiment to phosphorus is 145.1mg/g.
Example 2
The preparation method of the seawater modified biochar comprises the following steps:
(1) Cleaning fir tree branches, airing, crushing and grinding to obtain fir tree branch powder for later use;
(2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
(3) Putting fir branch powder into a crucible, wrapping tin foil paper on a crucible opening, covering a crucible cover, putting into a muffle furnace, starting heating, and keeping the temperature from room temperature to 600 ℃ for 2 hours at a heating rate of 10 ℃/min to enable the fir branch powder to be pyrolyzed into fir biochar;
(4) Mixing 0.2g of fir charcoal and 1L of filtered seawater, stirring at 250rpm for 0.5h, then dropwise adding 1mol/L NaOH solution into the mixture to adjust the pH value of the fir charcoal/seawater mixture to 10.50, then continuing stirring for 0.5h, and then standing the mixture at 30 ℃ for constant temperature aging for 16h;
(5) Filtering the aged mixture, collecting solid, washing the solid with pure water until the filtrate is neutral, drying at 60 ℃, grinding and sieving to obtain the seawater modified biochar.
The seawater modified biochar prepared in the embodiment is used as an adsorbent for treating phosphorus-containing wastewater with the phosphorus concentration of 97.5 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 5.0 by HCl or NaOH, 1g of adsorbent is added into 1L of phosphorus-containing wastewater, and the mixture is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 36.0mg/L, and the adsorption capacity of the seawater modified biochar prepared in the embodiment to phosphorus is 61.5mg/g.
Example 3
The preparation method of the seawater modified biochar comprises the following steps:
(1) Cleaning fir tree branches, airing, crushing and grinding to obtain fir tree branch powder for later use;
(2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
(3) Putting fir branch powder into a crucible, wrapping tin foil paper on a crucible opening, covering a crucible cover, putting into a muffle furnace, starting heating, and keeping the temperature from room temperature to 600 ℃ for 2 hours at a heating rate of 10 ℃/min to enable the fir branch powder to be pyrolyzed into fir biochar;
(4) Mixing 3g of fir charcoal with 1L of filtered seawater, stirring at 250rpm for 1h, then dropwise adding 3mol/L NaOH solution into the mixture to adjust the pH value of the fir charcoal/seawater mixture to 10.50, continuing stirring for 1h, and standing the mixture at 80 ℃ for constant temperature aging for 16h;
(5) Filtering the aged mixture, collecting solid, washing the solid with pure water until the filtrate is neutral, drying at 80 ℃, grinding and sieving to obtain the seawater modified biochar.
The seawater modified biochar prepared in the embodiment is used as an adsorbent for treating phosphorus-containing wastewater with the phosphorus concentration of 97.5 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 5.0 by HCl or NaOH, 1g of adsorbent is added into 1L of wastewater, and the wastewater is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 41.0mg/L, and the adsorption capacity of the seawater modified biochar prepared in the embodiment to phosphorus is 56.5mg/g.
Example 4
The preparation method of the seawater modified biochar comprises the following steps:
(1) Cleaning fir tree branches, airing, crushing and grinding to obtain fir tree branch powder for later use;
(2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
(3) Putting fir branch powder into a crucible, wrapping tin foil paper on a crucible opening, covering a crucible cover, putting into a muffle furnace, starting heating, and keeping the temperature from room temperature to 600 ℃ for 2 hours at a heating rate of 10 ℃/min to enable the fir branch powder to be pyrolyzed into fir biochar;
(4) Mixing 2g of fir charcoal with 1L of filtered seawater, stirring at 250rpm for 1h, then dropwise adding 1mol/L NaOH solution into the mixture to adjust the pH value of the fir charcoal/seawater mixture to 10.00, continuing stirring for 1h, and standing the mixture at 40 ℃ for constant temperature aging for 8h;
(5) Filtering the aged mixture, collecting solid, washing the solid with pure water until the filtrate is neutral, drying at 105 ℃, grinding and sieving to obtain the seawater modified biochar.
The seawater modified biochar prepared in the embodiment is used as an adsorbent for treating phosphorus-containing wastewater with the phosphorus concentration of 95.1 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 3.0 by HCl or NaOH, 0.5g of adsorbent is added into 1L of wastewater, and the wastewater is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 93.5mg/L, and the adsorption capacity of the seawater modified biochar prepared in the embodiment to phosphorus is 3.19mg/g.
Example 5
The preparation method of the seawater modified biochar comprises the following steps:
(1) Cleaning fir tree branches, airing, crushing and grinding to obtain fir tree branch powder for later use;
(2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
(3) Putting fir branch powder into a crucible, wrapping tin foil paper on a crucible opening, covering a crucible cover, putting into a muffle furnace, starting heating, and keeping the temperature from room temperature to 600 ℃ for 2 hours at a heating rate of 10 ℃/min to enable the fir branch powder to be pyrolyzed into fir biochar;
(4) Mixing 2g of fir charcoal with 1L of filtered seawater, stirring at 250rpm for 1h, then dropwise adding 1mol/L NaOH solution into the mixture to adjust the pH value of the fir charcoal/seawater mixture to 11.00, continuing stirring for 1h, and standing the mixture at 40 ℃ for constant temperature aging for 12h;
(5) Filtering the aged mixture, collecting solid, washing the solid with pure water until the filtrate is neutral, drying at 80 ℃, grinding and sieving to obtain the seawater modified biochar.
The seawater modified biochar prepared in the embodiment is used as an adsorbent for treating phosphorus-containing wastewater with the phosphorus concentration of 95.1 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 3.0 by HCl or NaOH, 0.5g of adsorbent is added into 1L of wastewater, and the wastewater is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 44.0mg/L, and the adsorption capacity of the seawater modified biochar prepared in the embodiment to phosphorus is 102.1mg/g.
Example 6
The preparation method of the seawater modified biochar comprises the following steps:
(1) Cleaning, airing, crushing and grinding corn stalks to obtain corn stalk powder for later use;
(2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
(3) Putting corn stalk powder into a crucible, wrapping tin foil paper on a crucible opening, covering a crucible cover, putting into a muffle furnace, starting heating, and keeping the temperature from room temperature to 600 ℃ for 2 hours at a heating rate of 10 ℃/min to enable the corn stalk powder to be pyrolyzed into corn stalk biochar;
(4) Mixing 2g of corn stalk charcoal with 1L of filtered seawater, stirring at 250rpm for 1h, then dropwise adding 1mol/L NaOH solution into the mixture to adjust the pH value of the corn stalk charcoal/seawater mixture to 10.50, continuing stirring for 1h, and standing the mixture at 40 ℃ for constant temperature aging for 12h;
(5) Filtering the aged mixture, collecting solid, washing the solid with pure water until the filtrate is neutral, drying at 80 ℃, grinding and sieving to obtain the seawater modified biochar.
The seawater modified biochar prepared in the embodiment is used as an adsorbent for treating the phosphorus-containing wastewater with the phosphorus concentration of 98.6 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 4.0 by HCl or NaOH, 0.5g of adsorbent is added into 1L of wastewater, and the wastewater is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 31.6mg/L, and the adsorption capacity of the seawater modified biochar prepared in the embodiment to phosphorus is 134.0mg/g.
Example 7
The preparation method of the seawater modified biochar comprises the following steps:
(1) Washing, airing, crushing and grinding vancomycin residues with the water content of 60-70% to obtain vancomycin residues powder for later use;
(2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
(3) Taking pure water as a solvent, wherein the filling degree is 50%, putting 5g of vancomycin fungus dreg powder into a hydrothermal reaction kettle, adding 50mL of pure water, adjusting the temperature to 140 ℃, and keeping the temperature for 15 hours to enable the vancomycin fungus dreg powder to be carbonized into vancomycin fungus dreg biochar;
(4) Mixing 2g of vancomycin fungus dreg charcoal and 1L of filtered seawater, stirring for 1h at 250rpm, then dropwise adding 1mol/L NaOH solution into the mixture to adjust the pH value of the mixture of the vancomycin fungus dreg charcoal/seawater to 10.50, then continuing stirring for 1h, and then standing the mixture at 40 ℃ for constant temperature aging for 12h;
(5) Filtering the aged mixture, collecting solid, washing the solid with pure water until the filtrate is neutral, drying at 80 ℃, grinding and sieving to obtain the seawater modified biochar.
The seawater modified biochar prepared in the embodiment is used as an adsorbent for treating phosphorus-containing wastewater with the phosphorus concentration of 95.74 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 3.0 by HCl or NaOH, 0.5g of adsorbent is added into 1L of wastewater, and the wastewater is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 34.6mg/L, and the adsorption capacity of the seawater modified biochar prepared in the embodiment to phosphorus is 103.0mg/g.
Example 8
The preparation method of the seawater modified biochar comprises the following steps:
(1) Washing, airing, crushing and grinding vancomycin residues with the water content of 60-70% to obtain vancomycin residues powder for later use;
(2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
(3) Taking pure water as a solvent, wherein the filling degree is 50%, putting 3g of vancomycin fungus dreg powder into a hydrothermal reaction kettle, adding 50mL of pure water, adjusting the temperature to 220 ℃, and keeping the temperature for 15 hours to enable the vancomycin fungus dreg powder to be carbonized into vancomycin fungus dreg biochar in a hydrothermal manner;
(4) Mixing 2g of vancomycin fungus dreg charcoal and 1L of filtered seawater, stirring for 1h at 250rpm, then dropwise adding 1mol/L NaOH solution into the mixture to adjust the pH value of the mixture of the vancomycin fungus dreg charcoal/seawater to 10.50, then continuing stirring for 1h, and then standing the mixture at 40 ℃ for constant temperature aging for 12h;
(5) Filtering the aged mixture, collecting solid, washing the solid with pure water until the filtrate is neutral, drying at 80 ℃, grinding and sieving to obtain the seawater modified biochar.
The seawater modified biochar prepared in the embodiment is used as an adsorbent for treating the phosphorus-containing wastewater with the phosphorus concentration of 102.6 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 5.0 by HCl or NaOH, 1g of adsorbent is added into 1L of wastewater, and the wastewater is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 35.4mg/L, and the adsorption capacity of the seawater modified biochar prepared in the embodiment to phosphorus is 67.2mg/g.
Comparative example 1
This comparative example provides a fir wood charcoal obtained by performing the procedure of step (1) → (2) → (3) in example 1.
The fir biochar prepared in the comparative example is used as an adsorbent for treating phosphorus-containing wastewater with the phosphorus concentration of 98.5 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 3.0 by HCl or NaOH, 0.5g of adsorbent is added into 1L of wastewater, and the wastewater is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 97.3mg/L, and the adsorption capacity of the fir biochar prepared in the comparative example on phosphorus is 2.40mg/g.
Comparative example 2
This comparative example provides a corn stover biochar obtained by performing the procedure of step (1) → (2) → (3) of example 6.
The corn stalk biochar prepared in the comparative example is used as an adsorbent for treating phosphorus-containing wastewater with the phosphorus concentration of 95.74 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 3.0 by HCl or NaOH, 0.5g of adsorbent is added into 1L of wastewater, and the wastewater is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 97.3mg/L, and the adsorption capacity of the corn stalk biochar prepared in the comparative example on phosphorus is-7.96 mg/g.
Comparative example 3
This comparative example provides a vancomycin residue biochar obtained by performing the procedure of step (1) → (2) → (3) in example 7.
The vancomycin fungus dreg biochar prepared in the comparative example is used as an adsorbent to treat phosphorus-containing wastewater with the phosphorus concentration of 102.5 mg/L: the pH value of the phosphorus-containing wastewater is regulated to 5.0 by HCl or NaOH, 1g of adsorbent is added into 1L of wastewater, and the wastewater is oscillated for 24 hours at a constant temperature of 25 ℃.
Through the steps, the phosphorus concentration in the phosphorus-containing wastewater is reduced to 100.5mg/L, and the adsorption capacity of the vancomycin fungus dreg biochar prepared in the comparative example on phosphorus is 2.00mg/g.
As can be seen from comparative examples 1-3, the adsorption capacity of the fir biochar, the corn stalk biochar and the vancomycin fungi residue biochar prepared in comparative examples 1-3 to phosphorus is weak, and the adsorption capacity is lower than 5mg/g; the corn stalk biochar not only does not adsorb but also releases phosphorus, so that the adsorption capacity of the corn stalk biochar to phosphorus is negative.
FIG. 1 is a scanning electron microscope image of fir charcoal prepared in comparative example 1. As can be seen from fig. 1, the fir wood charcoal has a smooth surface and is in a large-size block shape. FIG. 2 is a scanning electron microscope image of the seawater-modified biochar prepared in example 1, i.e., the seawater-modified biochar obtained by modifying the fir wood biochar prepared in comparative example 1 with seawater. As can be seen from fig. 2, the seawater-modified biochar surface is loaded with a large number of nano-sheets and a small number of irregular crystals. The nano-sheet is identified as Mg (OH) 2 The irregular crystal is CaCO 3 . Illustrating the modification process, mg in sea water 2+ And Ca 2+ Respectively with Mg (OH) 2 Nanoplatelets and CaCO 3 Loading of crystal forms toBiochar surface.
Comparing examples 1 to 8 with comparative examples 1 to 3, it can be seen that the adsorption capacity of the biochar can be greatly improved by modifying the biochar with seawater. In particular, under the optimal preparation condition (example 1), the adsorption capacity of the seawater modified biochar provided by the invention on phosphorus in water body can be up to 145.1mg/g, which is far higher than that of other common adsorption materials (such as active carbon, mineral materials and the like) and calcium/magnesium modified biochar reported in literature. Therefore, the seawater modified biochar provided by the invention has a good adsorption effect on phosphorus in a water body.
It should be understood that the embodiments and examples discussed herein are for illustrative purposes only and that modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the purview of this application and are to be included within the scope of the appended claims.
Claims (3)
1. A preparation method of seawater modified biochar is characterized by comprising the following steps of: the method comprises the following steps:
1) Cleaning, airing, crushing and grinding biomass to obtain biomass powder for later use;
2) Filtering natural seawater with 0.45 μm filter membrane to remove impurities;
3) Preparing biomass powder into biochar by adopting a pyrolysis method or a hydrothermal method;
4) Mixing biochar and filtered seawater according to the proportion of 0.2-3:1000 g/L, stirring, then dropwise adding alkali liquor to adjust the pH value of the biochar/seawater mixture to 10.5-11, continuing stirring, and standing the mixture for constant-temperature aging;
5) Filtering the aged mixture, collecting solids, washing the solids, drying, grinding and sieving to obtain seawater modified biochar, wherein Mg is contained in seawater 2+ And Ca 2+ Respectively with Mg (OH) 2 Nanoplatelets and CaCO 3 The crystal form is loaded on the surface of the biochar;
in the step 1), the biomass is any one of agricultural and forestry waste and antibiotic residues; the agricultural and forestry waste is any one of fir branches and corn stalks; the antibiotic fungus residues are vancomycin fungus residues with the water content of 60-70%;
in step 3), the pyrolysis method is as follows: placing biomass powder in a crucible, placing in a muffle furnace, starting heating, and keeping the temperature from room temperature to 600 ℃ for 2 hours at a heating rate of 10 ℃/min to enable the biomass powder to be pyrolyzed into biochar at a high temperature; the hydrothermal method comprises the following steps: 3-5 g of biomass powder is put into a hydrothermal reaction kettle by taking pure water as a solvent and the filling degree is 50%, 50mL of pure water is added, the temperature is regulated to 140-220 ℃, and the temperature is kept for 15 hours, so that the biomass powder is carbonized into biochar in a hydrothermal manner;
in the step 4), the alkali liquor is NaOH solution with the concentration of 1-3 mol/L; the aging condition is 30-80 ℃ for 8-16 h;
in the step 5), the drying temperature is 60-105 ℃.
2. A seawater-modified biochar produced by the production method of claim 1.
3. Use of the seawater-modified biochar according to claim 2 for adsorbing phosphorus.
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| CN107603649A (en) * | 2017-10-25 | 2018-01-19 | 华中科技大学 | A kind of preparation method of rich ketone bio oil and rich magnesium activated carbon |
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| CN111821950A (en) * | 2020-08-18 | 2020-10-27 | 湘潭大学 | Preparation method of biochar ammonia adsorbent |
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| CN110681350A (en) * | 2019-09-19 | 2020-01-14 | 天津大学 | Preparation method of phosphoric acid modified enteromorpha biological carbon and application of phosphoric acid modified enteromorpha biological carbon in removal of heavy metal cadmium |
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| CN107365593A (en) * | 2017-09-07 | 2017-11-21 | 中国科学院城市环境研究所 | A kind of method that antibiotic bacterium dregs prepare charcoal |
| CN107603649A (en) * | 2017-10-25 | 2018-01-19 | 华中科技大学 | A kind of preparation method of rich ketone bio oil and rich magnesium activated carbon |
| CN109499542A (en) * | 2019-01-20 | 2019-03-22 | 郗丹 | A kind of preparation method and application of the modification biological carbon composite of magnetic hydrotalcite modification |
| CN111001388A (en) * | 2019-12-30 | 2020-04-14 | 中国科学院城市环境研究所 | Preparation method and application of bamboo-based biochar phosphorus removal adsorbent |
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