CN105598158A - Phosphorus-based biochar material, and preparation and application thereof - Google Patents
Phosphorus-based biochar material, and preparation and application thereof Download PDFInfo
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- CN105598158A CN105598158A CN201610063992.1A CN201610063992A CN105598158A CN 105598158 A CN105598158 A CN 105598158A CN 201610063992 A CN201610063992 A CN 201610063992A CN 105598158 A CN105598158 A CN 105598158A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/10—Reclamation of contaminated soil microbiologically, biologically or by using enzymes
- B09C1/105—Reclamation of contaminated soil microbiologically, biologically or by using enzymes using fungi or plants
Abstract
The invention discloses a phosphorus-based biochar material, and preparation and application thereof. The phosphorus-based biochar material with a special structure and a special function is formed by performing anoxia high-temperature carbonization on mycelium pellets which are wrapped with nano hydroxyapatite and serve as a raw material. The synthesized phosphorus-based biochar material is uniformly mixed with soil according to a certain ratio to obtain a mixture; and after the mixture is cured for 7 days, the content of cadmium in an effective state in the soil is reduced by 44.8 to 50.1 percent, so that the treatment effect of the phosphorus-based biochar material is better than that of a pure-phosphorus-based material. The material preparation process is simple, and the cost is lower; biological degradation can be realized, and no secondary pollution is caused; and therefore, the phosphorus-based biochar material is an environment-friendly material.
Description
Technical field
The invention belongs to heavy metal-polluted soil recovery technique field, be specifically related to a kind of phosphorus base biological carbon materials andPreparation method, and adopt this phosphorus base biological carbon materials to administer the application process of cadmium pollution soil.
Background technology
In the recent period, be detected cadmium with the multiple batches of rice in the many provinces headed by Hunan and exceed standard, frequently existing " cadmium rice "Event, has pushed soil heavy metal cadmium to the teeth of the storm again. Cadmium is the heavy metal unit that bio-toxicity is the strongestOne of element, chemism in soil is strong, toxicity is lasting, easily by the enrichment harm of food chainHuman health. Soil heavy metal cadmium situation is very severe, the national soil pollution that announce in April, 2014The demonstration of status investigation communique, the some position exceeding standard rate of cadmium is the highest, is formally confirmed as the primary pollution of Chinese soilThing, administers and control technology in the urgent need to effective Cadmium Pollution in Soils.
Heavy Metal Pollution Control especially Some Mining Districts heavy metal pollution of soil reparation problem is around worldwideEnvironmental pollution improvement's difficult problem, has been subjected to domestic and international experts and scholars' extensive concern. At present, research soil weightThe governance way of metallic pollution mainly contains 2 aspects: the one, and taking the total amount of cutting down heavy metal in soil as object,Pollutant is removed from soil, transferred to another place by pollutant from soil; The 2nd, to change heavilyThe exist form of metal in soil is object, by pollutant passivation, changes into from soluble state or exchangeable speciesIndissoluble state, thus its animal migration and bioavailability in soil reduced. That relatively commonly uses both at home and abroad locatesReason means have physics reparation, chemical reparation, biological restoration, agronomic measures reparation etc. Every kind of recovery technique allThere are its pluses and minuses. Such as soil replacement method and soil moved in to improve the original method are applicable to the small size soil of serious pollution, quantities is large,Expense is high; Electronic repairing method is still in the experimental study stage, and energy consumption is large, and cost of investment is high; Chemical leaching methodDestructible soil physico-chemical property; Curing/stabilizing method treatment effect is determined according to fixative, and has certain ringBorder risk; Biological restoration is easy and simple to handle, harmless to soil, also non-secondary pollution, but repairing efficiency is long,Be not suitable for high density pollution soil yet. Therefore, need exploitation a kind of good fixing effect, lasting effect badly strong, rightThe renovation agent that soil physico-chemical property impact is less.
Phosphorus sill can not only improve crop yield, the effectively weight in fixing soil by as fertilizer sourcesMetal, be a kind of cheap, repair efficient soil fixing agent. Utilize the high transverse and longitudinal ratio of filamentous fungi and toolThere is the characteristic of biological viscosity etc., will there is the nano hydroxyapatite of high-specific surface area, high reaction activity and strong absorptionLime stone (n-HAP) is carried on mycelium, makes the mycelium pellet that is embedded with n-HAP. This fixative solvesThe n-HAP problem of too disperseing in soil, easily running off, but the more difficult soil remediation that applies to quantitativelyIn, also need to do a large amount of improvement apart from commercial Application.
Charcoal has flourishing pore structure because of it, and a large amount of functional groups and negative electrical charge, counterweight are contained in surfaceMetal ion has stronger absorption and crystallized ability, and can, by changing soil physico-chemical property, strengthen soilThe complexing power of earth to heavy metal cadmium, reduces Cadmium Pollution in Soils degree effectively, alleviates heavy metal raw to cropLong toxic action. Aspect control and improvement Cadmium Pollution in Soils, having broad application prospects. Therefore, knotClose both advantages, how will be embedded with the mycelium pellet of n-HAP and the environmental activity of charcoal is combined, preparationGo out phosphorus base charcoal composite, significant.
Summary of the invention
The object of the present invention is to provide a kind of phosphorus base biological carbon materials and preparation method thereof with it at cadmium pollution soilApplication in earth improvement, the fixing repairing effect of this phosphorus base biological carbon materials is good, and cost is lower, preparation and applicationMethod is simple, does not affect soil physico-chemical property, and crops are had no side effect, and uses safety.
For achieving the above object, the technical solution used in the present invention is:
A preparation method for phosphorus base biological carbon materials, comprises the following steps:
(1) adopt culture medium activation and expand cultivation filamentous fungi, for subsequent use;
(2) hydroxyapatite nano particle is added in fluid nutrient medium and disperseed;
(3) nano particle and medium sterilization processing;
(4), in ultra-clean aseptic operating platform, the mycelium that has activated and cultivated in step (1) is seeded toIn the sterilising medium of step (3);
(5) mycelium pellet that in step (4), vaccinated culture medium shaken cultivation forms.
(6) take out the mycelium pellet in step (5), put into after oven for drying its pyrolysis carbonization.
Filamentous fungi described in step (1) is that a class is thread, grows thickly, and has the fungi of high transverse and longitudinal ratio, bagDraw together aspergillus and/or mould.
Step adds hydroxyapatite nano particle in fluid nutrient medium in (2), and solid-to-liquid ratio is 0.1-2g:100-200mL, described hydroxyapatite nano particle, requires particle diameter < 100nm, purity > 97%; Adopt superSound disperses, power 50-100 watt, ultrasonic oscillation 0.5-3h.
Described in step (3), sterilization treatment is that the culture medium of hydroxyl phosphorite nano particle is put into sterilizingIn pot, arrange 115 DEG C, sterilizing 25min; After autoclave sterilization, the training of hydroxyl phosphorite nano particleFoster base is put into ultra-clean aseptic operating platform, opens uviol lamp sterilizing 30-90min.
In step (4), inoculative proportion is nanometer hydroxyapatite: fluid nutrient medium: bacterium liquid=0.1-2g:100-200mL:0.5-3mL, in bacterium liquid, mycelium mass concentration is 5.5-6mg/mL.
Step (5) is by the rotating speed 140-180rpm bar at 26-35 DEG C of vaccinated culture medium in step (4)Under part, cultivate 2-4 days.
Step (5) was cultivated after 2-4 days, was placed on matter with after the mycelium pellet of deionized water rinse formation 2-5 timeIn the glutaraldehyde of amount concentration 2.5-5%, at 4 DEG C, preserve.
In step (6), be placed on for 2-5 time in culture dish with deionized water rinse mycelium pellet, put into 50-60 DEG C of bakingCase is dried 1-2 days.
RESEARCH OF PYROCARBON described in step (6) turns to puts into 30-50mL porcelain crucible by the mycelium pellet of oven dry, add a cover,Put into the high temperature process furnances that is connected with nitrogen, it is 120-300 DEG C/h that heating rate is set, carburizing temperature 280-600DEG C, temperature retention time 2-4h.
A kind of phosphorus base biological carbon materials is to be prepared from by described method.
The application of described phosphorus base biological carbon materials, for the reparation of cadmium pollution soil.
The concrete application process of described phosphorus base biological carbon materials in cadmium pollution soil is administered, cadmium pollution soilAdd described phosphorus base biological carbon materials, then add deionized water, mass ratio is soil: the biological raw material of wood-charcoal of phosphorus baseMaterial: water=100:(1-5): (100-300), mix at least 7 days processing times.
The present invention has following advantage:
1. the present invention is taking the mycelium pellet that is embedded with nanometer hydroxyapatite as raw material, by anoxic high temperature cabonization, shapeBecome to have the phosphorus base biological carbon materials of special construction and function, fully combine filamentous fungi (high transverse and longitudinal ratio,There is biological viscosity), nanometer hydroxyapatite (high-specific surface area, high reaction activity, absorption by force) and biologicalCharcoal (having advantages of that a large amount of microcellular structures and huge specific area, adsorption capacity are stronger), has solvedThe problem that n-HAP too disperses, easily runs off in soil, also can put in contaminated soil easily.
2. the present invention selects filamentous fungi mycelia as load. As aspergillus niger be in aspergillus fungi one normalSee kind, wide material sources, are the type specimens that generally acknowledged filamentous fungi is studied. Mycelia production cost is extremely low, mistakeCheng Qingjie is sustainable, and processing, without expensive equipment, is convenient to large-scale production.
3. the present invention's material centered by nanometer hydroxyapatite, adopts aspergillus niger mycelia parcel nano-hydroxy-apatiteStone, then by anoxic high temperature cabonization, make the phosphorus base biological carbon materials of repairing for contaminated soil. Its featureMainly being that phosphorus base biological carbon materials adds enters after cadmium pollution soil, and the part cadmium in soil is inhaled by charcoalAttached, on the other hand, the hydroxyapatite slowly releasing dissolves gradually in the soil liquid, Cd2+With hydroxylCa in apatite2+There is ion-exchange, or by the adsorption of metal ions in hydroxyapatite surface lattice,By cadmium from the biologically effective state that is easy to be absorbed by organism to low activity Morphological Transitions. In addition, this material propertyStable, the nano-grade hydroxy apatite powder being wrapped up by charcoal discharges slowly, can keep long-term effectivelyProperty, and phosphorus burst size is little, can not cause body eutrophication.
4. the synthetic phosphorus base biological carbon materials of the present invention, under the equal prerequisite that uses nano material, more economical haveEffect. Under the prerequisite of same repairing effect, the nano material use amount in phosphorus base biological carbon materials is than simpleThe use amount that applies nano material will be lacked.
5. the synthetic phosphorus base biological carbon materials of the present invention is environment-friendly material, essential element consist of calcium, phosphorus,Carbon. Charcoal can improve soil physico-chemical property, accelerates edaphon metabolism, increases soil fertility. ?Nonhazardous in application process, biodegradable, non-secondary pollution.
Brief description of the drawings
Fig. 1 is the synthetic process chart of the embodiment of the present invention 1 phosphorus base biological carbon materials;
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of black-koji mould pompon of the present invention;
Fig. 3 is the scanning electron microscope (SEM) photograph (SEM) that the present invention is enclosed with n-HAP mycelium pellet (without charing);
Fig. 4 is the scanning electron microscope (SEM) photograph (SEM) of phosphorus base biological carbon materials of the present invention;
Detailed description of the invention
Be intended to the present invention to be described in further details below in conjunction with the drawings and specific embodiments, and unrestrictedInvention.
Embodiment 1
The phosphorus base biological carbon materials of preparation cadmium pollution soil repair of the present invention:
(1) adopt the activation of PDA culture medium and expand cultivation aspergillus niger (Aspergillusniger), in being purchased fromState's typical case's culture collection center, bacterium numbering CCTCCAF91006;
(2) hydroxyapatite nano particle of 1.0g (particle diameter < 100nm, purity > 97%) is added to 200mLLiquid PDA culture medium in, adopt the ultrasonic echography of 100 watts of power to disperse 2h;
(3) the PDA culture medium containing nanometer hydroxyapatite is put into high temperature high-pressure sterilizing pot, arranged115 DEG C, sterilizing 25min. After autoclave sterilization, media transfer, to ultra-clean aseptic operating platform, is opened purpleOuter lamp sterilizing 60min;
(4), in ultra-clean aseptic operating platform, the mycelium having activated in step (1) is seeded to step (3)Sterilising medium in, inoculum concentration is 2mL; In bacterium liquid, mycelium mass concentration is 5.89mg/mL;
(5) in step (4), vaccinated culture medium is placed in gas bath shaking table and vibrates, and cultivates 2-3 at 35 DEG CMy god, rotating speed is 150rpm;
(6) after 2-3 days, with the mycelium pellet forming in deionized water rinse step (5) 3 times, after be placed onIn the glutaraldehyde of mass concentration 2.5%, at 4 DEG C, preserve.
(7) draw one by one the mycelium pellet in glutaraldehyde solution with suction pipe, use deionized water rinse mycelium pellet 3 timesBe placed in culture dish, put into 60 DEG C of oven for drying 1 day.
(8) mycelium pellet of oven dry is put into 30mL porcelain crucible, add a cover, put into the high-temperature tubular that is connected with nitrogenStove, it is 300 DEG C/h that heating rate is set, 450 DEG C of carburizing temperatures, temperature retention time 2h.
(9) treat that furnace temperature drops to room temperature, take out sample, be product of the present invention.
Embodiment 2
Soil is taken from certain Pb-Zn tailings storehouse periphery low-pollution water rice soil. For examination soil reject after gravel and broken fromSo air-dry, quartering mixes, and pulverizes 18 order nylon mesh. Soil pH value is 6.58, is faintly acid. SoilIn earth, available state Cd content is 7.01mg/kg.
Respectively the phosphorus base biological carbon materials in 0.2g embodiment 1 (is measured and the pure n-HAP taking containing n-HAPAmount equates) add and enter in the low contaminated soil of 5.0g with pure n-HAP, mix, add the water of 10mL,Fix after 7 days, extract the available state of Cadmium in Soil with 25mLDTPA. After testing, low contaminated soil is through phosphorusBefore and after base biological carbon materials or pure n-HAP process, cadmium available state content is as shown in table 1 below.
The low contaminated soil of table 1 is processed front and back available state Cd content
| Available state Cd (mg/kg) | Fixed rate | |
| Low contaminated soil | 7.010 | — |
| After phosphorus base biological carbon materials is processed | 3.50 | 50.1％ |
| After pure n-HAP processes | 3.85 | 45.1％ |
Embodiment 3
Soil is taken from certain Pb-Zn tailings storehouse periphery intermediate pollution rice soil. Reject after gravel and broken for examination soilNatural air drying, quartering mixes, and pulverizes 18 order nylon mesh. Soil pH value is 6.52, is faintly acid.Soil available Cd content is 36.8mg/kg.
Respectively the phosphorus base biological carbon materials in 0.2g embodiment 1 (is measured and the pure n-HAP taking containing n-HAPAmount equates) add and enter in 5.0g in contaminated soil with pure n-HAP, mix, add the water of 10mL,Fix after 7 days, extract the available state of Cadmium in Soil with 25mLDTPA. After testing, middle contaminated soil is through phosphorusBefore and after base biological carbon materials or pure n-HAP process, cadmium available state content is as shown in table 2 below.
In table 2, contaminated soil is processed front and back available state Cd content
Embodiment 4
Soil is taken from certain Pb-Zn tailings storehouse periphery rice soil. Reject natural air drying after gravel and broken for examination soil,Quartering mixes, and pulverizes 18 order nylon mesh. Soil pH value is 5.90, is acid. Soil availableCd content is respectively 127.0mg/kg, and compared with embodiment 2,3, acidity obviously increases, and pollution level is non-Chang Chong, is called high pollution soil.
Respectively the phosphorus base biological carbon materials in 0.2g embodiment 1 (is measured and the pure n-HAP taking containing n-HAPAmount equates) add and enter in 5.0g high pollution soil with pure n-HAP, mix, add the water of 10mL,Fix after 7 days, extract the available state of Cadmium in Soil with 25mLDTPA. After testing, high pollution soil is through phosphorusBefore and after base biological carbon materials or pure n-HAP process, cadmium available state content is as shown in table 3 below.
Available state Cd content before and after table 3 high pollution soil treatment
| Available state Cd (mg/kg) | Fixed rate Cd | |
| High pollution soil | 127.0 | — |
| After phosphorus base biological carbon materials is processed | 70.1 | 44.8％ |
| After pure n-HAP processes | 93.6 | 26.3％ |
Claims (10)
1. a preparation method for phosphorus base biological carbon materials, is characterized in that, comprises the following steps:
(1) adopt culture medium activation and expand cultivation filamentous fungi, for subsequent use;
(2) hydroxyapatite nano particle is added in fluid nutrient medium and disperseed;
(3) nano particle and medium sterilization processing;
(4), in ultra-clean aseptic operating platform, the mycelium that has activated and cultivated in step (1) is seeded toIn the sterilising medium of step (3);
(5) mycelium pellet that in step (4), vaccinated culture medium shaken cultivation forms;
(6) take out the mycelium pellet in step (5), put into after oven for drying its pyrolysis carbonization.
2. preparation method according to claim 1, is characterized in that, thread described in step (1)Fungi is that a class is thread, grows thickly, and has the fungi of high transverse and longitudinal ratio, comprises aspergillus and/or mould.
3. preparation method according to claim 1, is characterized in that, in step (2) by hydroxyl phosphorusLime stone nano particle adds in fluid nutrient medium, and solid-to-liquid ratio is 0.1-2g:100-200mL, described hydroxy-apatiteStone nano particle, requires particle diameter < 100nm, purity > 97%; Adopt ultrasonic dispersion, power 50-100 watt,Ultrasonic oscillation 0.5-3h.
4. preparation method according to claim 1, is characterized in that, inoculative proportion in step (4)For nanometer hydroxyapatite: fluid nutrient medium: bacterium liquid=0.1-2g:100-200mL:0.5-3mL, in bacterium liquidMycelium mass concentration is 5.5-6mg/mL.
5. preparation method according to claim 1, is characterized in that, step (5) is by step (4)In vaccinated culture medium at 26-35 DEG C, under rotating speed 140-180rpm condition, cultivate 2-4 days.
6. preparation method according to claim 1, is characterized in that, step (5) was cultivated after 2-4 days,After mycelium pellet 2-5 time forming with deionized water rinse, be placed in the glutaraldehyde of mass concentration 2.5-5% in 4At DEG C, preserve.
7. preparation method according to claim 1, is characterized in that, step is used deionization in (6)Water rinse mycelium pellet is placed on for 2-5 time in culture dish, puts into 50-60 DEG C of oven for drying 1-2 days.
8. preparation method according to claim 1, is characterized in that, the heat described in step (6)Separating carbonization is that the mycelium pellet of oven dry is put into 30-50mL porcelain crucible, adds a cover, and puts into the high-temperature pipe that is connected with nitrogenFormula stove, it is 120-300 DEG C/h that heating rate is set, carburizing temperature 280-600 DEG C, temperature retention time 2-4h.
9. a phosphorus base biological carbon materials, is characterized in that, is by the side described in claim 1-8 any oneMethod is prepared from.
10. the application of phosphorus base biological carbon materials claimed in claim 9, is characterized in that, for cadmium pollutionThe reparation of soil.
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| CN109622014A (en) * | 2018-12-12 | 2019-04-16 | 安徽大学 | A kind of preparation method of the catalyst of electro-catalysis oxygen generation hydrogen peroxide |
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| CN110699348A (en) * | 2019-06-28 | 2020-01-17 | 北京林业大学 | Phosphorus-containing microbial capsule and preparation method and application thereof |
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| CN110373196B (en) * | 2019-07-31 | 2021-02-02 | 湖南农业大学 | Tobacco planting soil nano cadmium passivator and preparation method and application thereof |
| CN111349445A (en) * | 2020-04-02 | 2020-06-30 | 汤彪 | Slow-release repairing agent for soil pollution and preparation method thereof |
| CN111349445B (en) * | 2020-04-02 | 2021-07-09 | 山东省神农生态科技股份有限公司 | Slow-release repairing agent for soil pollution and preparation method thereof |
| CN114259987A (en) * | 2021-12-28 | 2022-04-01 | 辽宁大学 | Peanut shell/hydroxyapatite composite material, preparation method thereof and application thereof in Pb (II) adsorption separation |
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